##############################################################################
#                                                                            #
# This CIF contains the data for a data article accepted for                 #
# publication in IUCrData. It conforms to the requirements of                #
# Notes for Authors for IUCrData, and has been                               #
# peer reviewed under the auspices of IUCrData.                              #
#                                                                            #
# 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 data    # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_systematic
;\
Decacarbonyl(μ-ethylidenimino-1κN:2κC)-μ-hydrido-\
triangulo-triosmium(3 Os--Os)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C12 H5 N O10 Os3'
_chemical_formula_sum     'C12 H5 N O10 Os3'
_chemical_formula_iupac     '[Os3 (C2 H4 N) H (C O)10]'
_chemical_formula_weight     893.77
_chemical_melting_point     ?
_chemical_absolute_configuration     ad
_space_group_crystal_system     orthorhombic
_space_group_name_H-M_alt     'P 21 21 21'
_space_group_name_Hall     'P 2ac 2ab'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z+1/2'
    'x+1/2, -y+1/2, -z'
_cell_length_a     9.56470(6)
_cell_length_b     11.59555(8)
_cell_length_c     15.61610(11)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     90
_cell_volume     1731.95(2)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     23076
_cell_measurement_theta_min     3.7850
_cell_measurement_theta_max     73.4550
_cell_measurement_temperature     100.00(10)
loop_
    _twin_individual_id
    _twin_individual_mass_fraction_refined
    1 0.535(16)
    2 0.465(16)
_exptl_crystal_description     plate
_exptl_crystal_colour     'clear reddish orange'
_exptl_crystal_size_max     0.153
_exptl_crystal_size_mid     0.073
_exptl_crystal_size_min     0.023
_exptl_crystal_density_diffrn     3.428
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     1568
_exptl_absorpt_coefficient_mu     41.178
_exptl_absorpt_correction_type     gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_absorpt_correction_T_min     0.10920
_exptl_absorpt_correction_T_max     1.00000
_diffrn_ambient_temperature     100.00(10)
_diffrn_source     'micro-focus sealed X-ray tube'
_diffrn_radiation_type     CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator     mirror
_diffrn_measurement_device_type     'Rigaku SuperNova AtlasS2 CCD'
_diffrn_measurement_device     'four-circle diffractometer'
_diffrn_measurement_method     'ω scans'
_diffrn_detector     'CCD plate'
_diffrn_detector_area_resol_mean     5.2387
_diffrn_reflns_number     33313
_diffrn_reflns_av_R_equivalents     0.0518
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_theta_min     4.750
_diffrn_reflns_theta_max     73.577
_diffrn_reflns_theta_full     67.684
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -19
_diffrn_reflns_limit_l_max     19
_diffrn_radiation_probe     x-ray
_refine_special_details
;
An AFIX command was used to constrain the N-bound H atom. A DFIX command was
 used to constrain the position of hydride H atom.
;
_reflns_number_total     3487
_reflns_number_gt     3471
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0153
_refine_ls_R_factor_gt     0.0152
_refine_ls_wR_factor_gt     0.0368
_refine_ls_wR_factor_ref     0.0368
_refine_ls_goodness_of_fit_ref     1.060
_refine_ls_restrained_S_all     1.060
_refine_ls_number_reflns     3487
_refine_ls_number_parameters     241
_refine_ls_number_restraints     2
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
; w=1/[σ²(Fo²)+(0.0177P)²+1.9300P] where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary     ?
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.580
_refine_diff_density_min     -0.891
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack     0.465(16)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0181 0.0091
                         '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'
    'N' 'N' 0.0311 0.0180
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0492 0.0322
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Os' 'Os' -4.9801 6.2216
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_structure_solution     ?
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
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
    Os Os1 0.55519(3) 0.47729(2) 0.31968(2) 0.01492(7) Uani d 1 . .
    Os Os3 0.81319(3) 0.37203(2) 0.37293(2) 0.01544(7) Uani d 1 . .
    Os Os2 0.81157(3) 0.61402(2) 0.33737(2) 0.01578(7) Uani d 1 . .
    O O8 0.7118(6) 0.1256(5) 0.4066(3) 0.0295(12) Uani d 1 . .
    O O2 0.2816(6) 0.6049(5) 0.2863(3) 0.0265(11) Uani d 1 . .
    N N1 0.6712(6) 0.6362(5) 0.4404(3) 0.0192(11) Uani d 1 . .
    H H1 0.687362 0.682623 0.483836 0.023 Uiso calc 1 . .
    O O6 1.0711(6) 0.6239(5) 0.4504(3) 0.0270(11) Uani d 1 . .
    O O5 0.7938(6) 0.8712(4) 0.2948(4) 0.0309(12) Uani d 1 . .
    O O1 0.5513(7) 0.3569(5) 0.1421(3) 0.0317(12) Uani d 1 . .
    O O7 0.8601(5) 0.3331(4) 0.1797(3) 0.0218(10) Uani d 1 . .
    O O9 1.1229(6) 0.3324(6) 0.4109(4) 0.0375(15) Uani d 1 . .
    O O3 0.4224(6) 0.2725(5) 0.4103(4) 0.0355(13) Uani d 1 . .
    O O4 0.9924(5) 0.5754(5) 0.1790(3) 0.0246(11) Uani d 1 . .
    C C8 0.7491(7) 0.2157(7) 0.3941(4) 0.0237(15) Uani d 1 . .
    C C1 0.5576(8) 0.4015(6) 0.2072(4) 0.0235(14) Uani d 1 . .
    O O10 0.7542(6) 0.4424(5) 0.5608(3) 0.0292(12) Uani d 1 . .
    C C11 0.5588(8) 0.5746(6) 0.4332(4) 0.0179(13) Uani d 1 . .
    C C9 1.0074(8) 0.3481(7) 0.3968(5) 0.0254(16) Uani d 1 . .
    C C6 0.9740(8) 0.6201(6) 0.4085(5) 0.0225(15) Uani d 1 . .
    C C3 0.4709(7) 0.3493(7) 0.3761(5) 0.0238(16) Uani d 1 . .
    C C4 0.9231(7) 0.5866(6) 0.2380(4) 0.0199(14) Uani d 1 . .
    C C10 0.7726(7) 0.4187(6) 0.4916(4) 0.0209(15) Uani d 1 . .
    C C12 0.4450(8) 0.5834(7) 0.4983(4) 0.0259(15) Uani d 1 . .
    H H12A 0.363183 0.620690 0.472632 0.039 Uiso calc 1 . .
    H H12B 0.477705 0.629330 0.547069 0.039 Uiso calc 1 . .
    H H12C 0.419399 0.506005 0.518069 0.039 Uiso calc 1 . .
    C C5 0.7956(7) 0.7757(6) 0.3109(5) 0.0231(14) Uani d 1 . .
    C C7 0.8407(7) 0.3485(6) 0.2497(5) 0.0206(14) Uani d 1 . .
    C C2 0.3870(7) 0.5583(6) 0.2960(4) 0.0190(14) Uani d 1 . .
    H H2 0.652(9) 0.592(9) 0.273(6) 0.09(5) Uiso d 1 . .
_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
    Os1 Os3 . 2.8759(4) ?
    Os1 Os2 . 2.9331(4) ?
    Os1 C1 . 1.964(7) ?
    Os1 C11 . 2.102(6) ?
    Os1 C3 . 1.904(8) ?
    Os1 C2 . 1.899(7) ?
    Os1 H2 . 1.78(6) ?
    Os3 Os2 . 2.8604(4) ?
    Os3 C8 . 1.942(8) ?
    Os3 C9 . 1.914(8) ?
    Os3 C10 . 1.969(7) ?
    Os3 C7 . 1.961(7) ?
    Os2 N1 . 2.111(6) ?
    Os2 C6 . 1.911(7) ?
    Os2 C4 . 1.910(7) ?
    Os2 C5 . 1.926(7) ?
    Os2 H2 . 1.84(6) ?
    O8 C8 . 1.121(10) ?
    O2 C2 . 1.154(9) ?
    N1 H1 . 0.8800 ?
    N1 C11 . 1.296(10) ?
    O6 C6 . 1.137(9) ?
    O5 C5 . 1.136(9) ?
    O1 C1 . 1.142(9) ?
    O7 C7 . 1.124(9) ?
    O9 C9 . 1.142(10) ?
    O3 C3 . 1.138(9) ?
    O4 C4 . 1.141(9) ?
    O10 C10 . 1.128(9) ?
    C11 C12 . 1.493(10) ?
    C12 H12A . 0.9800 ?
    C12 H12B . 0.9800 ?
    C12 H12C . 0.9800 ?
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
    Os3 Os1 Os2 . . 58.988(9) ?
    Os3 Os1 H2 . . 89(3) ?
    Os2 Os1 H2 . . 37(2) ?
    C1 Os1 Os3 . . 93.4(2) ?
    C1 Os1 Os2 . . 108.4(2) ?
    C1 Os1 C11 . . 173.9(3) ?
    C1 Os1 H2 . . 88(4) ?
    C11 Os1 Os3 . . 88.3(2) ?
    C11 Os1 Os2 . . 67.5(2) ?
    C11 Os1 H2 . . 86(4) ?
    C3 Os1 Os3 . . 84.2(2) ?
    C3 Os1 Os2 . . 137.0(2) ?
    C3 Os1 C1 . . 94.0(3) ?
    C3 Os1 C11 . . 92.0(3) ?
    C3 Os1 H2 . . 173(2) ?
    C2 Os1 Os3 . . 173.2(2) ?
    C2 Os1 Os2 . . 117.3(2) ?
    C2 Os1 C1 . . 93.3(3) ?
    C2 Os1 C11 . . 85.0(3) ?
    C2 Os1 C3 . . 96.7(3) ?
    C2 Os1 H2 . . 90(3) ?
    Os2 Os3 Os1 . . 61.502(10) ?
    C8 Os3 Os1 . . 100.1(2) ?
    C8 Os3 Os2 . . 161.3(2) ?
    C8 Os3 C10 . . 92.0(3) ?
    C8 Os3 C7 . . 94.6(3) ?
    C9 Os3 Os1 . . 161.8(2) ?
    C9 Os3 Os2 . . 100.7(2) ?
    C9 Os3 C8 . . 97.9(3) ?
    C9 Os3 C10 . . 92.8(3) ?
    C9 Os3 C7 . . 92.3(3) ?
    C10 Os3 Os1 . . 89.2(2) ?
    C10 Os3 Os2 . . 85.0(2) ?
    C7 Os3 Os1 . . 83.7(2) ?
    C7 Os3 Os2 . . 86.9(2) ?
    C7 Os3 C10 . . 171.1(3) ?
    Os1 Os2 H2 . . 35(2) ?
    Os3 Os2 Os1 . . 59.509(9) ?
    Os3 Os2 H2 . . 88(3) ?
    N1 Os2 Os1 . . 66.78(15) ?
    N1 Os2 Os3 . . 88.56(16) ?
    N1 Os2 H2 . . 85(4) ?
    C6 Os2 Os1 . . 139.0(2) ?
    C6 Os2 Os3 . . 85.3(2) ?
    C6 Os2 N1 . . 94.0(3) ?
    C6 Os2 C5 . . 98.8(3) ?
    C6 Os2 H2 . . 174(2) ?
    C4 Os2 Os1 . . 107.5(2) ?
    C4 Os2 Os3 . . 89.5(2) ?
    C4 Os2 N1 . . 174.1(3) ?
    C4 Os2 C6 . . 91.4(3) ?
    C4 Os2 C5 . . 91.8(3) ?
    C4 Os2 H2 . . 90(4) ?
    C5 Os2 Os1 . . 116.1(2) ?
    C5 Os2 Os3 . . 175.6(2) ?
    C5 Os2 N1 . . 89.7(3) ?
    C5 Os2 H2 . . 87(3) ?
    Os2 N1 H1 . . 123.4 ?
    C11 N1 Os2 . . 113.3(4) ?
    C11 N1 H1 . . 123.4 ?
    O8 C8 Os3 . . 179.7(7) ?
    O1 C1 Os1 . . 176.3(7) ?
    N1 C11 Os1 . . 112.5(5) ?
    N1 C11 C12 . . 120.6(6) ?
    C12 C11 Os1 . . 126.8(5) ?
    O9 C9 Os3 . . 179.2(8) ?
    O6 C6 Os2 . . 179.6(7) ?
    O3 C3 Os1 . . 179.0(7) ?
    O4 C4 Os2 . . 176.7(6) ?
    O10 C10 Os3 . . 176.9(6) ?
    C11 C12 H12A . . 109.5 ?
    C11 C12 H12B . . 109.5 ?
    C11 C12 H12C . . 109.5 ?
    H12A C12 H12B . . 109.5 ?
    H12A C12 H12C . . 109.5 ?
    H12B C12 H12C . . 109.5 ?
    O5 C5 Os2 . . 176.3(7) ?
    O7 C7 Os3 . . 177.8(6) ?
    O2 C2 Os1 . . 175.8(6) ?
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
    Os2 N1 C11 Os1 . . . . -1.3(6) ?
    Os2 N1 C11 C12 . . . . -177.2(5) ?
_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.
;
_shelx_estimated_absorpt_T_min     0.062
_shelx_estimated_absorpt_T_max     0.451
data_global
_journal_date_recd_electronic     2019-09-09
_journal_date_accepted     2019-10-10
_journal_name_full     'IUCrData'
_journal_year     2019
_journal_volume     4
_journal_issue     10
_journal_page_first     0
_journal_page_last     0
_journal_paper_category     HM
_journal_paper_doi     10.1107/S2414314619013865
_journal_coeditor_code     WM4114
_publ_contact_author_name     'Cynthia B. Powell'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
Abilene Christian University
ACU 28132
Abilene, Texas 79699
USA
;
_publ_contact_author_email     powellc@acu.edu
_publ_contact_author_fax     ?
_publ_contact_author_phone     '325-674-2864'
_publ_section_title
;\
Decacarbonyl(μ-ethylidenimino-1κN:2κC)-μ-hydrido-\
triangulo-triosmium(3 Os--Os)
;
_publ_section_title_footnote     .
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Powell, Cynthia B.' .
;
Department of Chemistry and Biochemistry
Abilene Christian University
ACU 28132
Abilene, Texas 79699
USA
;
    'Powell, Gregory L.' .
;
Department of Chemistry and Biochemistry
Abilene Christian University
ACU 28132
Abilene, Texas 79699
USA
;
    'Archambeau, Ashley K. ' .
;
Department of Chemistry and Biochemistry
Abilene Christian University
ACU 28132
Abilene, Texas 79699
USA
;
    'Wilson, Kylie M.' .
;
Department of Chemistry and Biochemistry
Abilene Christian University
ACU 28132
Abilene, Texas 79699
USA
;
_publ_section_synopsis
;
The crystal structure of a new triosmium carbonyl complex containing bridging
ethylidenimino and hydrido ligands is reported. A relatively high-yield
synthesis was accomplished with the use of a triazine starting material and
microwave heating.
;
