##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
# http://www.iucr.org/resources/cif/software. #
# #
# This file may be used for bona fide research purposes within the #
# scientific community so long as proper attribution is given to the journal #
# article from which it was obtained. #
# #
##############################################################################
data_global
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_journal_data_validation_number ?
_journal_date_recd_electronic 2016-12-06
_journal_date_accepted 2017-01-26
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2017
_journal_volume 73
_journal_issue 3
_journal_page_first 318
_journal_page_last 321
_journal_paper_category GM
_journal_paper_doi 10.1107/S2056989017001360
_journal_coeditor_code ZS2371
loop_
_publ_contact_author_name
_publ_contact_author_address
_publ_contact_author_email
'Andrei I. Fischer'
;
Department of Inorganic Chemistry,
St Petersburg State Institute of Technology,
Moskovsky pr. 26, 190013, St Petersburg, Russian Federation
;
andreasfischer@mail.ru
'Vladislav V. Gurzhiy'
;
Institute of Earth Sciences, St Petersburg State University,
University Emb. 7/9, 199034, St Petersburg, Russian Federation
;
vladgeo17@mail.ru
_publ_contact_author_fax '7(812)712-77-91'
_publ_section_title
;\
Crystal structure of a Co^II^ coordination polymer:
catena-poly[[\m-aqua-bis(\m-2-methylpropanoato)-\k^2^O:\
O';\k^2^O:O-cobalt(II)] monohydrate]
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
'Andrei I. Fischer' .
;
St Petersburg State Institute of Technology,
Moskovsky pr. 26, 190013, St Petersburg, Russian Federation
;
'Vladislav V. Gurzhiy' .
;
Institute of Earth Sciences, St Petersburg State University,
University Emb. 7/9, 199034, St Petersburg, Russian Federation
;
'Julia V. Aleksandrova' .
;
St Petersburg State Institute of Technology,
Moskovsky pr. 26, 190013, St Petersburg, Russian Federation
;
'Maria I. Pakina' .
;
St Petersburg State Institute of Technology,
Moskovsky pr. 26, 190013, St Petersburg, Russian Federation
;
_publ_section_synopsis
;
The present paper describes the synthesis and crystal structure of a cobalt(II)
isobutyrate dihydrate, based on a slightly distorted CoO~6~ repeat unit
comprising four bridging carboxylate O-atom donors and two bridging water
donors, giving one-dimensional polymeric chains with composition
{[Co{(CH~3~)~2~CHCO~2~}~2~(H~2~O)]\\cdotH~2~O}~n~. Hydrogen bonding
through the water molecules gives two-dimensional sheets lying parallel to
(100).
;
_shelxl_version_number .2013
data_I
_database_code_depnum_ccdc_archive 'CCDC 1529830'
_chemical_name_systematic
;\
catena-Poly[[\m-aqua-bis(\m-2-methylpropanoato)-\
\k^2^O:O';\k^2^O:O-cobalt(II)] monohydrate]
;
_chemical_name_common 'cobalt(II) isobutyrate dihydrate'
_chemical_formula_moiety 'C8 H16 Co O5, H2 O'
_chemical_formula_sum 'C8 H18 Co O6'
_chemical_formula_iupac '[Co (C4 H7 O2)2 (H2 O)], H2 O'
_chemical_formula_weight 269.15
_chemical_melting_point ?
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 11.9999(4)
_cell_length_b 6.3815(2)
_cell_length_c 16.1374(6)
_cell_angle_alpha 90
_cell_angle_beta 109.540(2)
_cell_angle_gamma 90
_cell_volume 1164.59(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9959
_cell_measurement_theta_min 3.46
_cell_measurement_theta_max 49.60
_cell_measurement_temperature 100(2)
_cell_special_details ?
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'red'
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.1
_exptl_crystal_density_diffrn 1.535
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 564
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.075
-1 0 0 0.075
0 1 0 0.175
0 -1 0 0.175
0 0 1 0.050
0 0 -1 0.050
_exptl_absorpt_coefficient_mu 1.480
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_T_min 0.3040
_exptl_absorpt_correction_T_max 0.4166
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 25308
_diffrn_reflns_av_R_equivalents 0.0698
_diffrn_reflns_theta_min 3.462
_diffrn_reflns_theta_max 34.997
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_standards_number 0
_refine_special_details ?
_reflns_number_total 5082
_reflns_number_gt 4459
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0300
_refine_ls_R_factor_gt 0.0259
_refine_ls_wR_factor_gt 0.0666
_refine_ls_wR_factor_ref 0.0680
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_restrained_S_all 1.030
_refine_ls_number_reflns 5082
_refine_ls_number_parameters 152
_refine_ls_number_restraints 4
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max_lt 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 1.245
_refine_diff_density_min -0.507
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Co' 'Co' 0.3494 0.9721
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2012 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2012)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.49462(2) 0.68360(2) 0.24090(2) 0.00839(4) Uani d 1 . .
O O1A 0.66165(5) 0.60756(10) 0.24434(4) 0.01230(11) Uani d 1 . .
O O2A 0.67317(6) 0.26293(11) 0.27311(4) 0.01275(11) Uani d 1 . .
O O1B 0.43294(5) 0.41595(10) 0.16212(4) 0.01065(11) Uani d 1 . .
O O2B 0.34759(6) 0.20179(10) 0.05000(4) 0.01437(12) Uani d 1 . .
O O1W 0.49903(6) 0.45171(10) 0.34088(4) 0.01116(11) Uani d 1 . .
H H1W1 0.4417(17) 0.463(3) 0.3540(16) 0.017 Uiso d 1 . .
H H1W2 0.5573(18) 0.505(3) 0.3843(15) 0.017 Uiso d 1 . .
O O2W 0.29615(6) 0.39794(11) 0.37156(4) 0.01612(12) Uani d 1 . .
H H2W1 0.2869(13) 0.290(2) 0.3380(10) 0.024 Uiso d 1 . .
H H2W2 0.3027(13) 0.344(2) 0.4235(8) 0.024 Uiso d 1 . .
C C1A 0.71817(7) 0.43527(13) 0.26448(5) 0.01045(14) Uani d 1 . .
C C2A 0.85034(8) 0.44468(14) 0.28101(6) 0.01530(15) Uani d 1 . .
H H2A 0.8621 0.5188 0.2314 0.018 Uiso calc 1 . .
C C3A 0.90702(9) 0.2299(2) 0.28691(9) 0.0292(2) Uani d 1 . .
H H3A1 0.9021 0.1576 0.3377 0.044 Uiso calc 1 . .
H H3A2 0.9885 0.2457 0.2917 0.044 Uiso calc 1 . .
H H3A3 0.8663 0.1508 0.2350 0.044 Uiso calc 1 . .
C C4A 0.90875(11) 0.5731(2) 0.36327(11) 0.0409(4) Uani d 1 . .
H H4A1 0.8738 0.7102 0.3563 0.061 Uiso calc 1 . .
H H4A2 0.9918 0.5855 0.3726 0.061 Uiso calc 1 . .
H H4A3 0.8976 0.5050 0.4130 0.061 Uiso calc 1 . .
C C1B 0.36124(7) 0.38036(14) 0.08390(5) 0.01115(14) Uani d 1 . .
C C2B 0.29432(9) 0.56464(14) 0.03069(6) 0.01593(16) Uani d 1 . .
H H2B 0.2944 0.6787 0.0714 0.019 Uiso calc 1 . .
C C3B 0.16552(9) 0.50628(19) -0.02026(7) 0.0238(2) Uani d 1 . .
H H3B1 0.1637 0.3970 -0.0616 0.036 Uiso calc 1 . .
H H3B2 0.1245 0.6271 -0.0512 0.036 Uiso calc 1 . .
H H3B3 0.1278 0.4583 0.0201 0.036 Uiso calc 1 . .
C C4B 0.35856(10) 0.64054(17) -0.03141(6) 0.02213(19) Uani d 1 . .
H H4B1 0.4358 0.6907 0.0025 0.033 Uiso calc 1 . .
H H4B2 0.3142 0.7519 -0.0676 0.033 Uiso calc 1 . .
H H4B3 0.3660 0.5265 -0.0680 0.033 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Co1 0.00921(6) 0.00625(7) 0.00890(5) 0.00009(3) 0.00197(4) -0.00013(3)
O1A 0.0120(3) 0.0092(3) 0.0155(3) 0.0012(2) 0.0043(2) 0.0020(2)
O2A 0.0116(3) 0.0097(3) 0.0164(3) 0.0002(2) 0.0040(2) 0.0016(2)
O1B 0.0120(3) 0.0083(3) 0.0091(2) 0.00017(19) 0.00020(19) -0.00006(17)
O2B 0.0182(3) 0.0100(3) 0.0114(3) 0.0011(2) 0.0003(2) -0.00154(19)
O1W 0.0129(3) 0.0097(3) 0.0104(2) -0.0009(2) 0.0032(2) -0.00094(18)
O2W 0.0229(3) 0.0121(3) 0.0144(3) -0.0006(2) 0.0076(2) -0.0006(2)
C1A 0.0106(3) 0.0103(4) 0.0103(3) 0.0002(2) 0.0032(2) 0.0001(2)
C2A 0.0105(3) 0.0139(4) 0.0217(4) -0.0002(3) 0.0057(3) 0.0017(3)
C3A 0.0138(4) 0.0223(6) 0.0489(7) 0.0050(4) 0.0071(4) -0.0045(5)
C4A 0.0179(5) 0.0483(9) 0.0492(8) -0.0048(5) 0.0013(5) -0.0285(6)
C1B 0.0123(3) 0.0107(4) 0.0093(3) 0.0010(3) 0.0022(2) 0.0000(2)
C2B 0.0209(4) 0.0117(4) 0.0114(3) 0.0047(3) 0.0004(3) 0.0006(3)
C3B 0.0187(4) 0.0263(6) 0.0210(4) 0.0078(4) -0.0005(3) 0.0026(3)
C4B 0.0326(5) 0.0146(4) 0.0179(4) -0.0008(4) 0.0067(4) 0.0039(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1A . 2.0449(6) y
Co1 O2A 2_655 2.0142(6) y
Co1 O1B . 2.1100(6) y
Co1 O1B 2_655 2.1198(6) y
Co1 O1W . 2.1768(6) y
Co1 O1W 2_655 2.1777(6) y
O1A C1A . 1.2755(10) ?
O2A C1A . 1.2533(10) ?
O1B C1B . 1.2878(9) ?
O2B C1B . 1.2510(11) ?
O1W H1W1 . 0.79(2) ?
O1W H1W2 . 0.88(2) ?
O2W H2W1 . 0.861(12) ?
O2W H2W2 . 0.884(11) ?
C1A C2A . 1.5191(12) ?
C2A H2A . 0.9800 ?
C2A C3A . 1.5187(15) ?
C2A C4A . 1.5176(16) ?
C3A H3A1 . 0.9600 ?
C3A H3A2 . 0.9600 ?
C3A H3A3 . 0.9600 ?
C4A H4A1 . 0.9600 ?
C4A H4A2 . 0.9600 ?
C4A H4A3 . 0.9600 ?
C1B C2B . 1.5179(12) ?
C2B H2B . 0.9800 ?
C2B C3B . 1.5340(14) ?
C2B C4B . 1.5329(14) ?
C3B H3B1 . 0.9600 ?
C3B H3B2 . 0.9600 ?
C3B H3B3 . 0.9600 ?
C4B H4B1 . 0.9600 ?
C4B H4B2 . 0.9600 ?
C4B H4B3 . 0.9600 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1A Co1 O1B . . 88.13(3) y
O1A Co1 O1B . 2_655 89.41(3) y
O1A Co1 O1W . . 92.18(3) y
O1A Co1 O1W . 2_655 88.29(3) y
O2A Co1 O1A 2_655 . 175.30(3) y
O2A Co1 O1B 2_655 . 89.99(3) y
O2A Co1 O1B 2_655 2_655 93.14(3) y
O2A Co1 O1W 2_655 . 91.70(3) y
O2A Co1 O1W 2_655 2_655 88.33(3) y
O1B Co1 O1B . 2_655 170.29(2) y
O1B Co1 O1W . . 79.22(2) y
O1B Co1 O1W 2_655 . 91.49(2) y
O1B Co1 O1W . 2_655 110.31(2) y
O1B Co1 O1W 2_655 2_655 78.99(2) y
O1W Co1 O1W . 2_655 170.46(2) y
C1A O1A Co1 . . 130.11(6) ?
C1A O2A Co1 . 2_645 131.28(6) ?
Co1 O1B Co1 . 2_645 98.44(2) ?
C1B O1B Co1 . . 135.89(6) ?
C1B O1B Co1 . 2_645 125.09(6) ?
Co1 O1W Co1 . 2_645 94.70(2) ?
Co1 O1W H1W1 . . 109.1(16) ?
Co1 O1W H1W1 2_645 . 116.6(14) ?
Co1 O1W H1W2 . . 98.2(15) ?
Co1 O1W H1W2 2_645 . 127.6(14) ?
H1W1 O1W H1W2 . . 106(2) ?
H2W1 O2W H2W2 . . 103.8(14) ?
O2A C1A O1A . . 124.94(8) ?
O2A C1A C2A . . 118.59(7) ?
O1A C1A C2A . . 116.46(7) ?
C1A C2A H2A . . 107.6 ?
C3A C2A C1A . . 113.25(8) ?
C3A C2A H2A . . 107.6 ?
C4A C2A C1A . . 108.94(8) ?
C4A C2A H2A . . 107.6 ?
C4A C2A C3A . . 111.50(9) ?
C2A C3A H3A1 . . 109.5 ?
C2A C3A H3A2 . . 109.5 ?
C2A C3A H3A3 . . 109.5 ?
H3A1 C3A H3A2 . . 109.5 ?
H3A1 C3A H3A3 . . 109.5 ?
H3A2 C3A H3A3 . . 109.5 ?
C2A C4A H4A1 . . 109.5 ?
C2A C4A H4A2 . . 109.5 ?
C2A C4A H4A3 . . 109.5 ?
H4A1 C4A H4A2 . . 109.5 ?
H4A1 C4A H4A3 . . 109.5 ?
H4A2 C4A H4A3 . . 109.5 ?
O1B C1B C2B . . 118.13(8) ?
O2B C1B O1B . . 122.42(8) ?
O2B C1B C2B . . 119.42(7) ?
C1B C2B H2B . . 108.3 ?
C1B C2B C3B . . 111.27(8) ?
C1B C2B C4B . . 109.15(8) ?
C3B C2B H2B . . 108.3 ?
C4B C2B H2B . . 108.3 ?
C4B C2B C3B . . 111.30(8) ?
C2B C3B H3B1 . . 109.5 ?
C2B C3B H3B2 . . 109.5 ?
C2B C3B H3B3 . . 109.5 ?
H3B1 C3B H3B2 . . 109.5 ?
H3B1 C3B H3B3 . . 109.5 ?
H3B2 C3B H3B3 . . 109.5 ?
C2B C4B H4B1 . . 109.5 ?
C2B C4B H4B2 . . 109.5 ?
C2B C4B H4B3 . . 109.5 ?
H4B1 C4B H4B2 . . 109.5 ?
H4B1 C4B H4B3 . . 109.5 ?
H4B2 C4B H4B3 . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Co1 O1A C1A C2A . . . . -166.13(6) ?
Co1 O1A C1A O2A . . . . 12.38(12) ?
O1A C1A C2A C3A . . . . -168.74(8) ?
O1A C1A C2A C4A . . . . 66.57(12) ?
O2A C1A C2A C3A . . . . 12.65(12) ?
O2A C1A C2A C4A . . . . -112.03(11) ?
Co1 O1B C1B O2B . . . . 173.93(6) ?
Co1 O1B C1B O2B 2_645 . . . -16.84(12) ?
Co1 O1B C1B C2B . . . . -4.15(12) ?
Co1 O1B C1B C2B 2_645 . . . 165.09(6) ?
O1B C1B C2B C3B . . . . -138.98(8) ?
O1B C1B C2B C4B . . . . 97.80(9) ?
O2B C1B C2B C3B . . . . 42.89(11) ?
O2B C1B C2B C4B . . . . -80.33(10) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1W1 O2W . 0.79(2) 1.907(19) 2.6638(10) 161(2) y
O1W H1W2 O2B 2_655 0.88(2) 1.79(2) 2.6206(9) 158(2) y
O2W H2W1 O1A 2_645 0.861(12) 2.012(13) 2.7967(9) 151.0(13) y
O2W H2W2 O2B 4_566 0.884(11) 1.952(12) 2.8087(9) 163.0(14) y
C2B H2B O2A 2_655 0.98 2.47 3.3094(11) 144 y
_iucr_refine_instructions_details
;
TITL mo_B110_0m in P21/c #14
REM reset to P21/c #14
CELL 0.71073 11.9999 6.3815 16.1374 90 109.54 90
ZERR 4 0.0004 0.0002 0.0006 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C O Co H
UNIT 32 24 4 72
EQIV $1 1-X,-0.5+Y,0.5-Z
EQIV $2 +X,-1.5-Y,0.5+Z
EQIV $3 1-X,0.5+Y,0.5-Z
DFIX 0.9 O6 H6a O6 H6b
DFIX 2.15 H6a H3a
DFIX 0.95 O6 H6b
L.S. 20
PLAN 20
HTAB O6 O4_$1
HTAB O6 O5_$2
HTAB C2 O1
HTAB O3 O6
HTAB O3 O5_$3
BOND $H
Htab
conf
fmap 2
acta
OMIT -4 70
REM
REM
REM
WGHT 0.036200
FVAR 0.44107
CO1 3 0.494618 -0.316402 0.240900 11.00000 0.00921 0.00625 =
0.00890 -0.00013 0.00197 0.00009
O1 2 0.326828 -0.237071 0.226886 11.00000 0.01162 0.00968 =
0.01645 -0.00158 0.00404 -0.00016
O2 2 0.432940 -0.584054 0.162119 11.00000 0.01198 0.00832 =
0.00914 -0.00006 0.00020 0.00017
O3 2 0.499026 -0.548288 0.340882 11.00000 0.01286 0.00972 =
0.01040 -0.00094 0.00323 -0.00086
O4 2 0.661653 -0.392438 0.244337 11.00000 0.01196 0.00919 =
0.01553 0.00195 0.00433 0.00118
O5 2 0.347589 -0.798214 0.049998 11.00000 0.01822 0.01000 =
0.01140 -0.00154 0.00032 0.00107
O6 2 0.296146 -0.602063 0.371559 11.00000 0.02286 0.01214 =
0.01442 -0.00058 0.00762 -0.00063
H6A 4 0.286903 -0.710158 0.338033 11.00000 -1.50000
H6B 4 0.302742 -0.655548 0.423496 11.00000 -1.50000
C1 1 0.361244 -0.619637 0.083903 11.00000 0.01232 0.01070 =
0.00934 -0.00002 0.00217 0.00105
C2 1 0.294318 -0.435364 0.030685 11.00000 0.02088 0.01167 =
0.01143 0.00055 0.00036 0.00472
AFIX 13
H2 4 0.294430 -0.321265 0.071359 11.00000 -1.20000
AFIX 0
C3 1 0.165522 -0.493723 -0.020255 11.00000 0.01873 0.02632 =
0.02098 0.00258 -0.00047 0.00781
AFIX 137
H3C 4 0.163702 -0.603018 -0.061565 11.00000 -1.50000
H3D 4 0.124497 -0.372935 -0.051217 11.00000 -1.50000
H3E 4 0.127765 -0.541738 0.020137 11.00000 -1.50000
AFIX 0
C4 1 0.358557 -0.359458 -0.031411 11.00000 0.03255 0.01463 =
0.01788 0.00387 0.00669 -0.00077
AFIX 137
H4A 4 0.435780 -0.309261 0.002504 11.00000 -1.50000
H4B 4 0.314155 -0.248113 -0.067594 11.00000 -1.50000
H4C 4 0.365968 -0.473462 -0.068033 11.00000 -1.50000
AFIX 0
C5 1 0.718166 -0.564729 0.264480 11.00000 0.01062 0.01025 =
0.01028 0.00014 0.00321 0.00020
C6 1 0.850345 -0.555325 0.281007 11.00000 0.01053 0.01389 =
0.02171 0.00174 0.00569 -0.00015
AFIX 13
H6 4 0.862126 -0.481175 0.231402 11.00000 -1.20000
AFIX 0
C7 1 0.907015 -0.770083 0.286913 11.00000 0.01375 0.02232 =
0.04887 -0.00447 0.00707 0.00496
AFIX 137
H7A 4 0.902061 -0.842444 0.337720 11.00000 -1.50000
H7B 4 0.988515 -0.754348 0.291747 11.00000 -1.50000
H7C 4 0.866293 -0.849210 0.235007 11.00000 -1.50000
AFIX 0
C8 1 0.908753 -0.426858 0.363269 11.00000 0.01790 0.04827 =
0.04916 -0.02845 0.00126 -0.00475
AFIX 137
H8A 4 0.873811 -0.289825 0.356265 11.00000 -1.50000
H8B 4 0.991805 -0.414512 0.372624 11.00000 -1.50000
H8C 4 0.897590 -0.494975 0.412954 11.00000 -1.50000
AFIX 0
H3A 4 0.441653 -0.536520 0.353976 11.00000 -1.50000
H3B 4 0.557303 -0.494756 0.384290 11.00000 -1.50000
HKLF 4
REM mo_B110_0m in P21/c #14
REM R1 = 0.0259 for 4459 Fo > 4sig(Fo) and 0.0300 for all 5082 data
REM 152 parameters refined using 4 restraints
END
WGHT 0.0362 0.0000
REM Instructions for potential hydrogen bonds
HTAB O6 O4_$1
HTAB O6 O5_$2
HTAB C2 O1
HTAB O3 O6
HTAB O3 O5_$3
REM Highest difference peak 1.245, deepest hole -0.507, 1-sigma level 0.077
Q1 1 0.4947 -0.2044 0.2413 11.00000 0.05 1.25
Q2 1 0.4989 -0.4303 0.2420 11.00000 0.05 1.12
Q3 1 0.5329 -0.3163 0.2200 11.00000 0.05 0.53
Q4 1 0.4554 -0.3274 0.2609 11.00000 0.05 0.52
Q5 1 0.7839 -0.5654 0.2690 11.00000 0.05 0.50
Q6 1 0.9098 -0.5081 0.3979 11.00000 0.05 0.46
Q7 1 0.3465 -0.4165 0.0101 11.00000 0.05 0.44
Q8 1 0.4556 -0.3151 0.2074 11.00000 0.05 0.43
Q9 1 0.3986 -0.5813 0.1288 11.00000 0.05 0.43
Q10 1 0.3354 -0.5210 0.0592 11.00000 0.05 0.42
Q11 1 0.3604 -0.7098 0.0651 11.00000 0.05 0.39
Q12 1 0.4323 -0.7036 0.1696 11.00000 0.05 0.39
Q13 1 0.4973 -0.4331 0.3299 11.00000 0.05 0.37
Q14 1 0.8802 -0.5012 0.3230 11.00000 0.05 0.36
Q15 1 0.8706 -0.6639 0.2813 11.00000 0.05 0.36
Q16 1 0.2928 -0.5009 0.3674 11.00000 0.05 0.35
Q17 1 0.4354 -0.4784 0.1589 11.00000 0.05 0.34
Q18 1 0.6255 -0.3175 0.2617 11.00000 0.05 0.34
Q19 1 0.5039 -0.6239 0.3110 11.00000 0.05 0.33
Q20 1 0.7050 -0.6595 0.2563 11.00000 0.05 0.33
REM The information below was added by Olex2.
REM
REM R1 = 0.0259 for 4459 Fo > 4sig(Fo) and 0.0300 for all 41589 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.25, deepest hole -0.51
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0300
REM R1_gt = 0.0259
REM wR_ref = 0.0680
REM GOOF = 1.028
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 41589
REM Reflections_gt = 4459
REM Parameters = n/a
REM Hole = -0.51
REM Peak = 1.25
REM Flack = n/a
;