#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:01 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179971 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/65/7026530.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7026530
loop_
_publ_author_name
'Jayarathne, Upul'
'Chandrasekaran, Perumalreddy'
'Jacobsen, Heiko'
'Mague, Joel T.'
'Donahue, James P.'
_publ_section_title
;
 A tungsten-mediated closed cycle of reactivity for the reduction of CO(2)
 to CO.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9662
_journal_page_last               9671
_journal_paper_doi               10.1039/c0dt00489h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C26 H26 Cl4 P2 W, C20 H30 Co'
_chemical_formula_sum            'C46 H56 Cl4 Co P2 W'
_chemical_formula_weight         1055.43
_chemical_name_systematic
;
Bis(η⁵-pentamethylcyclopentadienyl)cobalt(III) trans-
tetrachlorobis(methyldiphenylphosphine)tungstate(III)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.829(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.227(10)
_cell_length_b                   11.087(4)
_cell_length_c                   17.943(6)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.77
_cell_volume                     4391(3)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36325
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  0.6227
_exptl_absorpt_correction_T_min  0.4995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.209
_refine_diff_density_min         -2.849
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00050(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+42.7460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                5427
_reflns_number_total             5653
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0dt00489h.txt
_cod_data_source_block           jpd272_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4392(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7026530
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.7500 -0.2500 0.5000 0.01162(9) Uani 1 2 d S
Cl1 Cl 0.66778(5) -0.10596(9) 0.42369(8) 0.0174(2) Uani 1 1 d .
Cl2 Cl 0.74657(5) -0.24995(9) 0.63183(8) 0.0172(2) Uani 1 1 d .
P1 P 0.82785(5) -0.07991(9) 0.58205(8) 0.0126(2) Uani 1 1 d .
C1 C 0.8641(2) -0.0267(4) 0.5290(3) 0.0155(8) Uani 1 1 d .
C2 C 0.9266(2) -0.0126(4) 0.5770(4) 0.0224(9) Uani 1 1 d .
H2 H 0.9527 -0.0376 0.6393 0.027 Uiso 1 1 calc R
C3 C 0.9511(2) 0.0375(5) 0.5347(4) 0.0270(11) Uani 1 1 d .
H3 H 0.9937 0.0461 0.5679 0.032 Uiso 1 1 calc R
C4 C 0.9137(3) 0.0746(4) 0.4449(4) 0.0285(11) Uani 1 1 d .
H4 H 0.9306 0.1096 0.4163 0.034 Uiso 1 1 calc R
C5 C 0.8515(2) 0.0614(4) 0.3956(4) 0.0244(10) Uani 1 1 d .
H5 H 0.8259 0.0874 0.3335 0.029 Uiso 1 1 calc R
C6 C 0.8267(2) 0.0103(4) 0.4372(3) 0.0195(9) Uani 1 1 d .
H6 H 0.7841 0.0004 0.4031 0.023 Uiso 1 1 calc R
C7 C 0.80747(19) 0.0617(4) 0.6098(3) 0.0140(8) Uani 1 1 d .
C8 C 0.8226(3) 0.1741(4) 0.5947(4) 0.0262(11) Uani 1 1 d .
H8 H 0.8397 0.1796 0.5613 0.031 Uiso 1 1 calc R
C9 C 0.8133(3) 0.2792(5) 0.6278(4) 0.0299(12) Uani 1 1 d .
H9 H 0.8246 0.3553 0.6180 0.036 Uiso 1 1 calc R
C10 C 0.7876(2) 0.2720(4) 0.6746(3) 0.0223(10) Uani 1 1 d .
H10 H 0.7811 0.3430 0.6973 0.027 Uiso 1 1 calc R
C11 C 0.7713(3) 0.1603(5) 0.6884(4) 0.0296(12) Uani 1 1 d .
H11 H 0.7538 0.1552 0.7211 0.036 Uiso 1 1 calc R
C12 C 0.7801(2) 0.0565(5) 0.6552(4) 0.0256(10) Uani 1 1 d .
H12 H 0.7674 -0.0190 0.6634 0.031 Uiso 1 1 calc R
C13 C 0.8905(2) -0.1293(4) 0.6966(3) 0.0190(9) Uani 1 1 d .
H13A H 0.9108 -0.1983 0.6913 0.029 Uiso 1 1 calc R
H13B H 0.8749 -0.1531 0.7317 0.029 Uiso 1 1 calc R
H13C H 0.9195 -0.0631 0.7283 0.029 Uiso 1 1 calc R
Co1 Co 0.5000 1.0000 0.5000 0.01144(16) Uani 1 2 d S
C14 C 0.5022(2) 0.8407(4) 0.5595(3) 0.0202(9) Uani 1 1 d .
C15 C 0.5328(2) 0.8281(4) 0.5171(3) 0.0169(8) Uani 1 1 d .
C16 C 0.49046(19) 0.8561(4) 0.4214(3) 0.0135(8) Uani 1 1 d .
C17 C 0.43380(19) 0.8850(4) 0.4064(3) 0.0159(8) Uani 1 1 d .
C18 C 0.4414(2) 0.8749(4) 0.4917(3) 0.0185(9) Uani 1 1 d .
C19 C 0.5295(3) 0.8171(5) 0.6585(4) 0.0319(12) Uani 1 1 d .
H19A H 0.5159 0.7383 0.6648 0.048 Uiso 1 1 calc R
H19B H 0.5167 0.8801 0.6821 0.048 Uiso 1 1 calc R
H19C H 0.5737 0.8174 0.6937 0.048 Uiso 1 1 calc R
C20 C 0.5972(2) 0.7893(5) 0.5629(4) 0.0281(11) Uani 1 1 d .
H20A H 0.6222 0.8187 0.6264 0.042 Uiso 1 1 calc R
H20B H 0.6124 0.8228 0.5293 0.042 Uiso 1 1 calc R
H20C H 0.5992 0.7011 0.5627 0.042 Uiso 1 1 calc R
C21 C 0.5037(2) 0.8520(5) 0.3515(3) 0.0224(10) Uani 1 1 d .
H21A H 0.5039 0.7679 0.3347 0.034 Uiso 1 1 calc R
H21B H 0.5434 0.8883 0.3772 0.034 Uiso 1 1 calc R
H21C H 0.4725 0.8970 0.2966 0.034 Uiso 1 1 calc R
C22 C 0.3758(2) 0.9165(5) 0.3156(3) 0.0253(10) Uani 1 1 d .
H22A H 0.3850 0.9469 0.2738 0.038 Uiso 1 1 calc R
H22B H 0.3543 0.9787 0.3249 0.038 Uiso 1 1 calc R
H22C H 0.3504 0.8444 0.2891 0.038 Uiso 1 1 calc R
C23 C 0.3925(3) 0.8911(5) 0.5044(4) 0.0285(11) Uani 1 1 d .
H23A H 0.3672 0.9600 0.4679 0.043 Uiso 1 1 calc R
H23B H 0.4106 0.9059 0.5695 0.043 Uiso 1 1 calc R
H23C H 0.3676 0.8180 0.4844 0.043 Uiso 1 1 calc R
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 W1 Cl1 180.0 7_646 .
Cl1 W1 Cl2 90.05(4) 7_646 7_646
Cl1 W1 Cl2 89.96(4) . 7_646
Cl1 W1 Cl2 89.95(4) 7_646 .
Cl1 W1 Cl2 90.04(4) . .
Cl2 W1 Cl2 180.00(5) 7_646 .
Cl1 W1 P1 91.12(4) 7_646 7_646
Cl1 W1 P1 88.88(4) . 7_646
Cl2 W1 P1 86.01(4) 7_646 7_646
Cl2 W1 P1 93.99(4) . 7_646
Cl1 W1 P1 88.88(4) 7_646 .
Cl1 W1 P1 91.12(4) . .
Cl2 W1 P1 93.98(4) 7_646 .
Cl2 W1 P1 86.01(4) . .
P1 W1 P1 180.0 7_646 .
C1 P1 C13 104.5(2) . .
C1 P1 C7 102.0(2) . .
C13 P1 C7 100.6(2) . .
C1 P1 W1 117.16(15) . .
C13 P1 W1 109.86(16) . .
C7 P1 W1 120.50(14) . .
C2 C1 C6 118.5(4) . .
C2 C1 P1 123.5(4) . .
C6 C1 P1 117.8(3) . .
C3 C2 C1 120.7(5) . .
C3 C2 H2 119.6 . .
C1 C2 H2 119.6 . .
C4 C3 C2 120.0(5) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C3 C4 C5 120.4(5) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C4 C5 C6 119.9(5) . .
C4 C5 H5 120.1 . .
C6 C5 H5 120.1 . .
C5 C6 C1 120.4(4) . .
C5 C6 H6 119.8 . .
C1 C6 H6 119.8 . .
C8 C7 C12 118.4(4) . .
C8 C7 P1 123.0(3) . .
C12 C7 P1 118.4(3) . .
C7 C8 C9 121.0(5) . .
C7 C8 H8 119.5 . .
C9 C8 H8 119.5 . .
C10 C9 C8 119.8(5) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C10 C11 119.5(4) . .
C9 C10 H10 120.3 . .
C11 C10 H10 120.3 . .
C12 C11 C10 120.9(5) . .
C12 C11 H11 119.5 . .
C10 C11 H11 119.5 . .
C11 C12 C7 120.4(5) . .
C11 C12 H12 119.8 . .
C7 C12 H12 119.8 . .
P1 C13 H13A 109.5 . .
P1 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
P1 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C17 Co1 C17 179.999(1) . 5_676
C17 Co1 C16 138.73(16) . 5_676
C17 Co1 C16 41.27(16) 5_676 5_676
C17 Co1 C16 41.27(16) . .
C17 Co1 C16 138.73(16) 5_676 .
C16 Co1 C16 179.997(1) 5_676 .
C17 Co1 C14 111.61(19) . 5_676
C17 Co1 C14 68.39(19) 5_676 5_676
C16 Co1 C14 68.86(17) 5_676 5_676
C16 Co1 C14 111.14(17) . 5_676
C17 Co1 C14 68.39(19) . .
C17 Co1 C14 111.61(19) 5_676 .
C16 Co1 C14 111.14(17) 5_676 .
C16 Co1 C14 68.86(17) . .
C14 Co1 C14 180.0(3) 5_676 .
C17 Co1 C15 68.84(18) . .
C17 Co1 C15 111.16(18) 5_676 .
C16 Co1 C15 138.99(17) 5_676 .
C16 Co1 C15 41.01(17) . .
C14 Co1 C15 139.24(18) 5_676 .
C14 Co1 C15 40.76(18) . .
C17 Co1 C15 111.16(18) . 5_676
C17 Co1 C15 68.84(18) 5_676 5_676
C16 Co1 C15 41.00(17) 5_676 5_676
C16 Co1 C15 138.99(17) . 5_676
C14 Co1 C15 40.77(18) 5_676 5_676
C14 Co1 C15 139.23(18) . 5_676
C15 Co1 C15 180.0(3) . 5_676
C17 Co1 C18 139.27(18) . 5_676
C17 Co1 C18 40.73(18) 5_676 5_676
C16 Co1 C18 69.03(17) 5_676 5_676
C16 Co1 C18 110.97(17) . 5_676
C14 Co1 C18 40.40(19) 5_676 5_676
C14 Co1 C18 139.60(19) . 5_676
C15 Co1 C18 111.47(18) . 5_676
C15 Co1 C18 68.53(18) 5_676 5_676
C17 Co1 C18 40.73(18) . .
C17 Co1 C18 139.27(18) 5_676 .
C16 Co1 C18 110.97(17) 5_676 .
C16 Co1 C18 69.03(17) . .
C14 Co1 C18 139.60(19) 5_676 .
C14 Co1 C18 40.40(19) . .
C15 Co1 C18 68.53(18) . .
C15 Co1 C18 111.47(18) 5_676 .
C18 Co1 C18 179.999(1) 5_676 .
C18 C14 C15 108.6(4) . .
C18 C14 C19 126.0(5) . .
C15 C14 C19 125.3(5) . .
C18 C14 Co1 69.9(3) . .
C15 C14 Co1 69.7(3) . .
C19 C14 Co1 127.9(3) . .
C14 C15 C16 107.9(4) . .
C14 C15 C20 126.7(4) . .
C16 C15 C20 125.4(4) . .
C14 C15 Co1 69.5(3) . .
C16 C15 Co1 69.2(2) . .
C20 C15 Co1 128.0(3) . .
C15 C16 C17 107.1(4) . .
C15 C16 C21 125.4(4) . .
C17 C16 C21 127.4(4) . .
C15 C16 Co1 69.8(2) . .
C17 C16 Co1 69.2(2) . .
C21 C16 Co1 127.4(3) . .
C18 C17 C16 108.4(4) . .
C18 C17 C22 125.7(4) . .
C16 C17 C22 125.9(4) . .
C18 C17 Co1 70.2(2) . .
C16 C17 Co1 69.6(2) . .
C22 C17 Co1 127.6(3) . .
C14 C18 C17 108.0(4) . .
C14 C18 C23 126.8(4) . .
C17 C18 C23 125.1(5) . .
C14 C18 Co1 69.6(3) . .
C17 C18 Co1 69.1(2) . .
C23 C18 Co1 129.4(3) . .
C14 C19 H19A 109.5 . .
C14 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C14 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C15 C20 H20A 109.5 . .
C15 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C15 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C16 C21 H21A 109.5 . .
C16 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C16 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C18 C23 H23A 109.5 . .
C18 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C18 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 Cl1 2.4182(12) 7_646
W1 Cl1 2.4182(12) .
W1 Cl2 2.4213(13) 7_646
W1 Cl2 2.4214(13) .
W1 P1 2.5619(12) 7_646
W1 P1 2.5619(12) .
P1 C1 1.824(4) .
P1 C13 1.825(5) .
P1 C7 1.829(4) .
C1 C2 1.396(6) .
C1 C6 1.399(6) .
C2 C3 1.385(7) .
C2 H2 0.9500 .
C3 C4 1.372(8) .
C3 H3 0.9500 .
C4 C5 1.385(7) .
C4 H4 0.9500 .
C5 C6 1.386(6) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.389(6) .
C7 C12 1.389(6) .
C8 C9 1.398(7) .
C8 H8 0.9500 .
C9 C10 1.372(7) .
C9 H9 0.9500 .
C10 C11 1.386(7) .
C10 H10 0.9500 .
C11 C12 1.380(7) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
Co1 C17 2.037(4) .
Co1 C17 2.037(4) 5_676
Co1 C16 2.043(4) 5_676
Co1 C16 2.043(4) .
Co1 C14 2.047(5) 5_676
Co1 C14 2.048(5) .
Co1 C15 2.050(4) .
Co1 C15 2.050(4) 5_676
Co1 C18 2.052(5) 5_676
Co1 C18 2.052(5) .
C14 C18 1.416(7) .
C14 C15 1.427(6) .
C14 C19 1.493(7) .
C15 C16 1.433(6) .
C15 C20 1.501(6) .
C16 C17 1.438(6) .
C16 C21 1.496(6) .
C17 C18 1.423(6) .
C17 C22 1.502(6) .
C18 C23 1.488(6) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
