##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# 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 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. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
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##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Dichlorobis(triphenylphosphine oxide-\kO)nickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C36 H30 Cl2 Ni O2 P2'
_chemical_formula_sum     'C36 H30 Cl2 Ni O2 P2'
_chemical_formula_iupac     '[Ni Cl2 (C18 H15 O P)2]'
_chemical_formula_weight     686.15
_chemical_melting_point     463.0(10)
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'F d d 2'
_symmetry_space_group_name_Hall     'F 2 -2d'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z'
    '-x+1/4, y+1/4, z+1/4'
    'x+1/4, -y+1/4, z+1/4'
    'x, y+1/2, z+1/2'
    '-x, -y+1/2, z+1/2'
    '-x+1/4, y+3/4, z+3/4'
    'x+1/4, -y+3/4, z+3/4'
    'x+1/2, y, z+1/2'
    '-x+1/2, -y, z+1/2'
    '-x+3/4, y+1/4, z+3/4'
    'x+3/4, -y+1/4, z+3/4'
    'x+1/2, y+1/2, z'
    '-x+1/2, -y+1/2, z'
    '-x+3/4, y+3/4, z+1/4'
    'x+3/4, -y+3/4, z+1/4'
_cell_length_a     20.6356(3)
_cell_length_b     32.5388(6)
_cell_length_c     9.72400(10)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     6529.25(17)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     3709
_cell_measurement_theta_min     1.00
_cell_measurement_theta_max     27.47
_cell_measurement_temperature     123(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     pale_blue
_exptl_crystal_size_max     0.35
_exptl_crystal_size_mid     0.30
_exptl_crystal_size_min     0.15
_exptl_crystal_density_diffrn     1.396
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2832
_exptl_absorpt_coefficient_mu     0.888
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(DENZO; Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min     0.802
_exptl_absorpt_correction_T_max     0.868
_diffrn_ambient_temperature     123(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius KappaCCD'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     7169
_diffrn_reflns_av_R_equivalents     0.0205
_diffrn_reflns_av_sigmaI/netI     0.0303
_diffrn_reflns_theta_min     2.34
_diffrn_reflns_theta_max     27.47
_diffrn_reflns_theta_full     27.47
_diffrn_measured_fraction_theta_max     1.00
_diffrn_measured_fraction_theta_full     1.00
_diffrn_reflns_limit_h_min     -26
_diffrn_reflns_limit_h_max     26
_diffrn_reflns_limit_k_min     -42
_diffrn_reflns_limit_k_max     42
_diffrn_reflns_limit_l_min     -12
_diffrn_reflns_limit_l_max     12
_diffrn_standards_number     0
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     0
_reflns_number_total     3686
_reflns_number_gt     3468
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0296
_refine_ls_R_factor_gt     0.0260
_refine_ls_wR_factor_gt     0.0617
_refine_ls_wR_factor_ref     0.0631
_refine_ls_goodness_of_fit_ref     1.065
_refine_ls_restrained_S_all     1.065
_refine_ls_number_reflns     3686
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0304P)²+7.7683P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.453
_refine_diff_density_min     -0.292
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.00057(6)
_refine_ls_abs_structure_details     'Flack (1983)'
_refine_ls_abs_structure_Flack     0.0010(10)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'C' 'C' 0.0033 0.0016
                         '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
                   'DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 2000)'
_computing_cell_refinement     'DENZO and COLLECT'
_computing_data_reduction     'DENZO and COLLECT'
_computing_structure_solution     'SHELXS86 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material     SHELXL97
loop_
    _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_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni 0.2500 0.2500 0.0000 0.01108(9) Uani d S 1 . . Ni
    P 0.16831(3) 0.178349(16) 0.18060(7) 0.01842(12) Uani d . 1 . . P
    Cl 0.32802(3) 0.22015(2) -0.12042(7) 0.03064(14) Uani d . 1 . . Cl
    O1 0.21631(7) 0.21054(5) 0.13540(17) 0.0254(3) Uani d . 1 . . O
    C1 0.17605(10) 0.13228(7) 0.0797(2) 0.0212(4) Uani d . 1 . . C
    C2 0.12395(11) 0.10513(7) 0.0611(3) 0.0269(5) Uani d . 1 . . C
    H2 0.0837 0.1103 0.1052 0.032 Uiso calc R 1 . . H
    C3 0.13114(12) 0.07063(7) -0.0219(3) 0.0316(5) Uani d . 1 . . C
    H3 0.0959 0.0522 -0.0342 0.038 Uiso calc R 1 . . H
    C4 0.18974(12) 0.06317(7) -0.0865(2) 0.0298(5) Uani d . 1 . . C
    H4 0.1944 0.0399 -0.1447 0.036 Uiso calc R 1 . . H
    C5 0.24159(12) 0.08943(8) -0.0666(2) 0.0293(5) Uani d . 1 . . C
    H5 0.2819 0.0838 -0.1097 0.035 Uiso calc R 1 . . H
    C6 0.23510(10) 0.12386(7) 0.0153(2) 0.0247(5) Uani d . 1 . . C
    H6 0.2709 0.1418 0.0279 0.030 Uiso calc R 1 . . H
    C7 0.08511(10) 0.19434(6) 0.1652(2) 0.0199(4) Uani d . 1 . . C
    C8 0.04882(11) 0.20515(7) 0.2806(2) 0.0246(5) Uani d . 1 . . C
    H8 0.0677 0.2040 0.3696 0.030 Uiso calc R 1 . . H
    C9 -0.01545(10) 0.21768(7) 0.2646(3) 0.0290(5) Uani d . 1 . . C
    H9 -0.0402 0.2251 0.3431 0.035 Uiso calc R 1 . . H
    C10 -0.04314(10) 0.21945(7) 0.1362(3) 0.0269(5) Uani d . 1 . . C
    H10 -0.0870 0.2278 0.1267 0.032 Uiso calc R 1 . . H
    C11 -0.00720(10) 0.20909(7) 0.0201(2) 0.0262(5) Uani d . 1 . . C
    H11 -0.0264 0.2105 -0.0685 0.031 Uiso calc R 1 . . H
    C12 0.05715(11) 0.19661(7) 0.0343(2) 0.0239(5) Uani d . 1 . . C
    H12 0.0819 0.1897 -0.0447 0.029 Uiso calc R 1 . . H
    C13 0.18248(10) 0.16712(7) 0.3592(2) 0.0221(4) Uani d . 1 . . C
    C14 0.15370(12) 0.13430(7) 0.4272(3) 0.0304(5) Uani d . 1 . . C
    H14 0.1273 0.1154 0.3780 0.036 Uiso calc R 1 . . H
    C15 0.16364(14) 0.12914(9) 0.5678(3) 0.0394(6) Uani d . 1 . . C
    H15 0.1441 0.1066 0.6142 0.047 Uiso calc R 1 . . H
    C16 0.20120(16) 0.15620(9) 0.6391(3) 0.0447(7) Uani d . 1 . . C
    H16 0.2068 0.1528 0.7355 0.054 Uiso calc R 1 . . H
    C17 0.23141(18) 0.18867(9) 0.5724(3) 0.0477(8) Uani d . 1 . . C
    H17 0.2582 0.2071 0.6226 0.057 Uiso calc R 1 . . H
    C18 0.22245(14) 0.19416(8) 0.4323(3) 0.0361(6) Uani d . 1 . . C
    H18 0.2434 0.2162 0.3861 0.043 Uiso calc R 1 . . H
_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
    Ni O1 14 1.9661(15) ?
    Ni O1 . 1.9661(15) ?
    Ni Cl 14 2.2152(5) ?
    Ni Cl . 2.2152(5) ?
    P O1 . 1.5072(15) ?
    P C13 . 1.799(2) ?
    P C1 . 1.799(2) ?
    P C7 . 1.800(2) ?
    C1 C6 . 1.397(3) ?
    C1 C2 . 1.403(3) ?
    C2 C3 . 1.390(3) ?
    C2 H2 . 0.9500 ?
    C3 C4 . 1.384(4) ?
    C3 H3 . 0.9500 ?
    C4 C5 . 1.383(4) ?
    C4 H4 . 0.9500 ?
    C5 C6 . 1.381(3) ?
    C5 H5 . 0.9500 ?
    C6 H6 . 0.9500 ?
    C7 C8 . 1.394(3) ?
    C7 C12 . 1.399(3) ?
    C8 C9 . 1.396(3) ?
    C8 H8 . 0.9500 ?
    C9 C10 . 1.374(4) ?
    C9 H9 . 0.9500 ?
    C10 C11 . 1.392(3) ?
    C10 H10 . 0.9500 ?
    C11 C12 . 1.396(3) ?
    C11 H11 . 0.9500 ?
    C12 H12 . 0.9500 ?
    C13 C14 . 1.389(3) ?
    C13 C18 . 1.400(3) ?
    C14 C15 . 1.392(4) ?
    C14 H14 . 0.9500 ?
    C15 C16 . 1.363(4) ?
    C15 H15 . 0.9500 ?
    C16 C17 . 1.388(4) ?
    C16 H16 . 0.9500 ?
    C17 C18 . 1.386(4) ?
    C17 H17 . 0.9500 ?
    C18 H18 . 0.9500 ?
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
    O1 Ni O1 14 . 95.92(10) ?
    O1 Ni Cl 14 14 108.95(5) ?
    O1 Ni Cl . 14 112.54(5) ?
    O1 Ni Cl 14 . 112.54(5) ?
    O1 Ni Cl . . 108.95(5) ?
    Cl Ni Cl 14 . 116.17(3) ?
    O1 P C13 . . 108.42(10) ?
    O1 P C1 . . 111.20(10) ?
    C13 P C1 . . 110.06(10) ?
    O1 P C7 . . 113.68(9) ?
    C13 P C7 . . 107.11(10) ?
    C1 P C7 . . 106.27(10) ?
    P O1 Ni . . 151.84(10) ?
    C6 C1 C2 . . 119.1(2) ?
    C6 C1 P . . 119.05(17) ?
    C2 C1 P . . 121.80(17) ?
    C3 C2 C1 . . 120.1(2) ?
    C3 C2 H2 . . 120.0 ?
    C1 C2 H2 . . 120.0 ?
    C4 C3 C2 . . 119.9(2) ?
    C4 C3 H3 . . 120.1 ?
    C2 C3 H3 . . 120.1 ?
    C5 C4 C3 . . 120.3(2) ?
    C5 C4 H4 . . 119.9 ?
    C3 C4 H4 . . 119.9 ?
    C6 C5 C4 . . 120.5(2) ?
    C6 C5 H5 . . 119.8 ?
    C4 C5 H5 . . 119.8 ?
    C5 C6 C1 . . 120.1(2) ?
    C5 C6 H6 . . 119.9 ?
    C1 C6 H6 . . 119.9 ?
    C8 C7 C12 . . 119.81(19) ?
    C8 C7 P . . 121.21(16) ?
    C12 C7 P . . 118.96(16) ?
    C7 C8 C9 . . 119.6(2) ?
    C7 C8 H8 . . 120.2 ?
    C9 C8 H8 . . 120.2 ?
    C10 C9 C8 . . 120.6(2) ?
    C10 C9 H9 . . 119.7 ?
    C8 C9 H9 . . 119.7 ?
    C9 C10 C11 . . 120.3(2) ?
    C9 C10 H10 . . 119.8 ?
    C11 C10 H10 . . 119.8 ?
    C10 C11 C12 . . 119.8(2) ?
    C10 C11 H11 . . 120.1 ?
    C12 C11 H11 . . 120.1 ?
    C11 C12 C7 . . 119.9(2) ?
    C11 C12 H12 . . 120.1 ?
    C7 C12 H12 . . 120.1 ?
    C14 C13 C18 . . 119.6(2) ?
    C14 C13 P . . 123.11(18) ?
    C18 C13 P . . 117.28(18) ?
    C13 C14 C15 . . 119.8(2) ?
    C13 C14 H14 . . 120.1 ?
    C15 C14 H14 . . 120.1 ?
    C16 C15 C14 . . 120.4(3) ?
    C16 C15 H15 . . 119.8 ?
    C14 C15 H15 . . 119.8 ?
    C15 C16 C17 . . 120.6(3) ?
    C15 C16 H16 . . 119.7 ?
    C17 C16 H16 . . 119.7 ?
    C18 C17 C16 . . 119.8(3) ?
    C18 C17 H17 . . 120.1 ?
    C16 C17 H17 . . 120.1 ?
    C17 C18 C13 . . 119.8(3) ?
    C17 C18 H18 . . 120.1 ?
    C13 C18 H18 . . 120.1 ?
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
    C13 P O1 Ni . . . . -171.8(2) ?
    C1 P O1 Ni . . . . 67.1(2) ?
    C7 P O1 Ni . . . . -52.8(2) ?
    O1 Ni O1 P 14 . . . 148.4(3) ?
    Cl Ni O1 P 14 . . . 35.1(2) ?
    Cl Ni O1 P . . . . -95.3(2) ?
    O1 P C1 C6 . . . . 24.3(2) ?
    C13 P C1 C6 . . . . -95.91(19) ?
    C7 P C1 C6 . . . . 148.45(18) ?
    O1 P C1 C2 . . . . -154.12(18) ?
    C13 P C1 C2 . . . . 85.7(2) ?
    C7 P C1 C2 . . . . -29.9(2) ?
    C6 C1 C2 C3 . . . . -0.8(3) ?
    P C1 C2 C3 . . . . 177.60(18) ?
    C1 C2 C3 C4 . . . . -0.2(3) ?
    C2 C3 C4 C5 . . . . 1.3(4) ?
    C3 C4 C5 C6 . . . . -1.5(4) ?
    C4 C5 C6 C1 . . . . 0.4(3) ?
    C2 C1 C6 C5 . . . . 0.7(3) ?
    P C1 C6 C5 . . . . -177.74(18) ?
    O1 P C7 C8 . . . . -105.11(19) ?
    C13 P C7 C8 . . . . 14.6(2) ?
    C1 P C7 C8 . . . . 132.25(18) ?
    O1 P C7 C12 . . . . 73.65(19) ?
    C13 P C7 C12 . . . . -166.62(17) ?
    C1 P C7 C12 . . . . -49.0(2) ?
    C12 C7 C8 C9 . . . . 0.8(3) ?
    P C7 C8 C9 . . . . 179.55(17) ?
    C7 C8 C9 C10 . . . . 0.0(4) ?
    C8 C9 C10 C11 . . . . -0.6(4) ?
    C9 C10 C11 C12 . . . . 0.4(4) ?
    C10 C11 C12 C7 . . . . 0.4(3) ?
    C8 C7 C12 C11 . . . . -1.0(3) ?
    P C7 C12 C11 . . . . -179.76(17) ?
    O1 P C13 C14 . . . . -169.46(19) ?
    C1 P C13 C14 . . . . -47.6(2) ?
    C7 P C13 C14 . . . . 67.5(2) ?
    O1 P C13 C18 . . . . 13.3(2) ?
    C1 P C13 C18 . . . . 135.08(19) ?
    C7 P C13 C18 . . . . -109.8(2) ?
    C18 C13 C14 C15 . . . . 1.5(4) ?
    P C13 C14 C15 . . . . -175.8(2) ?
    C13 C14 C15 C16 . . . . 0.3(4) ?
    C14 C15 C16 C17 . . . . -1.6(5) ?
    C15 C16 C17 C18 . . . . 1.2(5) ?
    C16 C17 C18 C13 . . . . 0.6(5) ?
    C14 C13 C18 C17 . . . . -1.9(4) ?
    P C13 C18 C17 . . . . 175.5(3) ?
data_global
_journal_date_recd_electronic     2004-10-28
_journal_date_accepted     2004-11-10
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2004
_journal_volume     60
_journal_issue     12
_journal_page_first     m1861
_journal_page_last     m1862
_journal_paper_category     EM
_publ_contact_author_name     'Dr Rodolfo Moreno-Fuquen'
_publ_contact_author_address
;
Departamento de Química
Facultad de Ciencias
Universidad del Valle
Apartado 25360
Santiago de Cali
Colombia
;
_publ_contact_author_email     rodolfu@telesat.com.co
_publ_contact_author_fax     '57 23 392440'
_publ_contact_author_phone     '57 23 393248'
_publ_section_title
;
Dichlorobis(triphenylphosphine oxide-\kO)nickel(II)
;
loop_
    _publ_author_name
    _publ_author_address
    'Moreno-Fuquen, Rodolfo'
;
Departamento de Química
Facultad de Ciencias
Universidad del Valle
Apartado 25360
Santiago de Cali
Colombia
;
    'Cifuentes, Olga'
;
Departamento de Química
Facultad de Ciencias
Universidad del Valle
Apartado 25360
Santiago de Cali
Colombia
;
    'Valderrama Naranjo, Jaime'
;
Departamento de Física
Facultad de Ciencias
Universidad del Valle
Apartado 25360
Santiago de Cali,
Colombia
;
    'Serratto, Luis Manuel'
;
Departamento de Química
Facultad de Ciencias
Universidad del Valle
Apartado 25360
Santiago de Cali
Colombia
;
    'Kennedy, Alan R.'
;
Department of Pure and Applied Chemistry
University of Strathclyde
295 Cathedral Street
Glasgow G1 1XL
Scotland
;
