#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:01 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179971 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/65/7026528.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_7026528
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_sum            'C26 H26 Cl4 P2 W'
_chemical_formula_weight         726.06
_chemical_name_common
;
Bis(diphenylmethylphosphine)tungsten(IV) tetrachloride
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.983(4)
_cell_angle_beta                 89.510(4)
_cell_angle_gamma                63.041(4)
_cell_formula_units_Z            1
_cell_length_a                   8.860(3)
_cell_length_b                   9.491(3)
_cell_length_c                   9.765(3)
_cell_measurement_reflns_used    6029
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2885
_cell_measurement_theta_min      2.316
_cell_volume                     659.2(4)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2008a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2008a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.934
_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  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6008
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    4.922
_exptl_absorpt_correction_T_max  0.4711
_exptl_absorpt_correction_T_min  0.3896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 2008a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.400
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0152
_refine_ls_R_factor_gt           0.0152
_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)+(0.0232P)²+0.2164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0388
_reflns_number_gt                3047
_reflns_number_total             3047
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0dt00489h.txt
_cod_data_source_block           jpd154
_cod_original_cell_volume        659.3(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026528
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.5000 0.0000 1.0000 0.00867(4) Uani 1 2 d S
Cl1 Cl 0.27372(5) 0.27992(6) 0.94772(5) 0.01276(9) Uani 1 1 d .
Cl2 Cl 0.32611(6) -0.03126(6) 0.84662(5) 0.01435(9) Uani 1 1 d .
P1 P 0.39775(6) -0.14436(6) 1.23487(5) 0.00958(9) Uani 1 1 d .
C1 C 0.5735(3) -0.2843(3) 1.4009(2) 0.0143(4) Uani 1 1 d .
H1A H 0.621(3) -0.219(4) 1.420(3) 0.020(7) Uiso 1 1 d .
H1B H 0.539(4) -0.348(4) 1.489(3) 0.025(7) Uiso 1 1 d .
H1C H 0.666(4) -0.369(4) 1.377(3) 0.031(8) Uiso 1 1 d .
C2 C 0.3235(2) -0.2921(2) 1.2262(2) 0.0120(3) Uani 1 1 d .
C3 C 0.4279(3) -0.4235(3) 1.1822(2) 0.0154(4) Uani 1 1 d .
H3 H 0.532(4) -0.422(4) 1.147(3) 0.023(7) Uiso 1 1 d .
C4 C 0.3767(3) -0.5401(3) 1.1771(2) 0.0173(4) Uani 1 1 d .
H4 H 0.453(3) -0.629(4) 1.151(3) 0.019(6) Uiso 1 1 d .
C5 C 0.2203(3) -0.5267(3) 1.2143(2) 0.0176(4) Uani 1 1 d .
H5 H 0.184(4) -0.600(4) 1.205(3) 0.021(7) Uiso 1 1 d .
C6 C 0.1169(3) -0.3981(3) 1.2592(2) 0.0173(4) Uani 1 1 d .
H6 H 0.012(3) -0.390(3) 1.285(3) 0.014(6) Uiso 1 1 d .
C7 C 0.1673(2) -0.2809(3) 1.2652(2) 0.0147(4) Uani 1 1 d .
H7 H 0.091(3) -0.195(4) 1.296(3) 0.020(6) Uiso 1 1 d .
C8 C 0.2235(2) 0.0092(2) 1.2868(2) 0.0115(3) Uani 1 1 d .
C9 C 0.2432(3) 0.0182(3) 1.4244(2) 0.0137(4) Uani 1 1 d .
H9 H 0.356(3) -0.060(3) 1.500(3) 0.016(6) Uiso 1 1 d .
C10 C 0.1048(3) 0.1396(3) 1.4579(2) 0.0173(4) Uani 1 1 d .
H10 H 0.119(3) 0.143(3) 1.555(3) 0.018(6) Uiso 1 1 d .
C11 C -0.0532(3) 0.2502(3) 1.3558(2) 0.0174(4) Uani 1 1 d .
H11 H -0.151(4) 0.335(4) 1.377(3) 0.026(7) Uiso 1 1 d .
C12 C -0.0734(3) 0.2419(3) 1.2189(2) 0.0167(4) Uani 1 1 d .
H12 H -0.186(4) 0.320(4) 1.146(4) 0.030(8) Uiso 1 1 d .
C13 C 0.0642(3) 0.1234(3) 1.1832(2) 0.0141(4) Uani 1 1 d .
H13 H 0.047(3) 0.119(3) 1.086(3) 0.017(6) Uiso 1 1 d .
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'
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 2_657 .
Cl1 W1 Cl2 89.84(3) 2_657 2_657
Cl1 W1 Cl2 90.16(3) . 2_657
Cl1 W1 Cl2 90.16(3) 2_657 .
Cl1 W1 Cl2 89.84(3) . .
Cl2 W1 Cl2 180.000(1) 2_657 .
Cl1 W1 P1 92.10(2) 2_657 2_657
Cl1 W1 P1 87.90(2) . 2_657
Cl2 W1 P1 90.34(3) 2_657 2_657
Cl2 W1 P1 89.66(3) . 2_657
Cl1 W1 P1 87.90(2) 2_657 .
Cl1 W1 P1 92.10(2) . .
Cl2 W1 P1 89.66(3) 2_657 .
Cl2 W1 P1 90.34(3) . .
P1 W1 P1 180.0 2_657 .
C8 P1 C1 106.08(9) . .
C8 P1 C2 104.89(9) . .
C1 P1 C2 103.03(9) . .
C8 P1 W1 114.44(6) . .
C1 P1 W1 110.90(7) . .
C2 P1 W1 116.39(6) . .
C7 C2 C3 118.81(18) . .
C7 C2 P1 122.24(15) . .
C3 C2 P1 118.94(15) . .
C4 C3 C2 120.41(19) . .
C3 C4 C5 120.42(19) . .
C6 C5 C4 119.54(19) . .
C5 C6 C7 120.48(19) . .
C6 C7 C2 120.33(18) . .
C9 C8 C13 119.50(17) . .
C9 C8 P1 122.40(15) . .
C13 C8 P1 118.10(14) . .
C10 C9 C8 119.87(18) . .
C11 C10 C9 120.29(19) . .
C10 C11 C12 120.06(19) . .
C13 C12 C11 120.20(19) . .
C12 C13 C8 120.07(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 Cl1 2.3378(7) 2_657
W1 Cl1 2.3379(7) .
W1 Cl2 2.3466(6) 2_657
W1 Cl2 2.3466(6) .
W1 P1 2.5672(7) 2_657
W1 P1 2.5672(7) .
P1 C8 1.8140(19) .
P1 C1 1.817(2) .
P1 C2 1.827(2) .
C2 C7 1.400(3) .
C2 C3 1.401(3) .
C3 C4 1.389(3) .
C4 C5 1.392(3) .
C5 C6 1.386(3) .
C6 C7 1.393(3) .
C8 C9 1.397(3) .
C8 C13 1.403(3) .
C9 C10 1.394(3) .
C10 C11 1.389(3) .
C11 C12 1.387(3) .
C12 C13 1.389(3) .
