#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:01 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179971 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/65/7026533.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_7026533
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         'C28 H32 Cl3 N P2 W'
_chemical_formula_sum            'C28 H32 Cl3 N P2 W'
_chemical_formula_weight         734.69
_chemical_name_systematic
;
trans-Trichloro(dimethylamido)bis(methyldiphenylphosphine)
tungsten(IV)
;
_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                 93.997(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8088(8)
_cell_length_b                   13.2473(8)
_cell_length_c                   16.0074(9)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.43
_cell_volume                     2921.1(3)
_computing_cell_refinement       'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_collection       'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'Bruker SAINT (Bruker-AXS 2009a)'
_computing_molecular_graphics    'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24988
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    4.357
_exptl_absorpt_correction_T_max  0.7925
_exptl_absorpt_correction_T_min  0.6553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0124P)²+3.1402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0339
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                3269
_reflns_number_total             3526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00489h.txt
_cod_data_source_block           jpd349_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_sg_symbol_H-M      C2/c
_cod_database_code               7026533
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 0.5000 0.794647(8) 0.7500 0.01236(4) Uani 1 2 d S
Cl1 Cl 0.34860(3) 0.78926(3) 0.66744(3) 0.01676(9) Uani 1 1 d .
Cl2 Cl 0.5000 0.60970(5) 0.7500 0.01844(13) Uani 1 2 d S
P1 P 0.59888(4) 0.77569(4) 0.62117(3) 0.01483(10) Uani 1 1 d .
N1 N 0.5000 0.94020(16) 0.7500 0.0147(5) Uani 1 2 d S
C1 C 0.53572(14) 0.72945(14) 0.52515(12) 0.0174(4) Uani 1 1 d .
C2 C 0.45855(14) 0.78490(14) 0.48678(13) 0.0186(4) Uani 1 1 d .
H2 H 0.4400 0.8470 0.5107 0.022 Uiso 1 1 calc R
C3 C 0.40910(15) 0.74991(16) 0.41429(13) 0.0225(4) Uani 1 1 d .
H3 H 0.3574 0.7885 0.3884 0.027 Uiso 1 1 calc R
C4 C 0.43469(16) 0.65889(17) 0.37931(14) 0.0282(5) Uani 1 1 d .
H4 H 0.4006 0.6351 0.3296 0.034 Uiso 1 1 calc R
C5 C 0.51014(17) 0.60273(17) 0.41713(15) 0.0317(5) Uani 1 1 d .
H5 H 0.5275 0.5401 0.3935 0.038 Uiso 1 1 calc R
C6 C 0.56042(16) 0.63779(16) 0.48945(14) 0.0260(5) Uani 1 1 d .
H6 H 0.6122 0.5989 0.5149 0.031 Uiso 1 1 calc R
C7 C 0.66177(13) 0.89074(14) 0.59260(12) 0.0163(4) Uani 1 1 d .
C8 C 0.65983(14) 0.92809(14) 0.51135(12) 0.0176(4) Uani 1 1 d .
H8 H 0.6215 0.8954 0.4678 0.021 Uiso 1 1 calc R
C9 C 0.71383(15) 1.01312(15) 0.49356(13) 0.0205(4) Uani 1 1 d .
H9 H 0.7123 1.0380 0.4378 0.025 Uiso 1 1 calc R
C10 C 0.76978(15) 1.06170(15) 0.55647(13) 0.0213(4) Uani 1 1 d .
H10 H 0.8070 1.1194 0.5439 0.026 Uiso 1 1 calc R
C11 C 0.77125(15) 1.02563(16) 0.63800(13) 0.0225(4) Uani 1 1 d .
H11 H 0.8090 1.0592 0.6814 0.027 Uiso 1 1 calc R
C12 C 0.71790(15) 0.94098(15) 0.65634(13) 0.0212(4) Uani 1 1 d .
H12 H 0.7192 0.9167 0.7123 0.025 Uiso 1 1 calc R
C13 C 0.69998(15) 0.68912(15) 0.64221(13) 0.0224(4) Uani 1 1 d .
H13A H 0.7381 0.6851 0.5929 0.034 Uiso 1 1 calc R
H13B H 0.6750 0.6220 0.6549 0.034 Uiso 1 1 calc R
H13C H 0.7413 0.7137 0.6902 0.034 Uiso 1 1 calc R
C14 C 0.47102(15) 1.00473(15) 0.67785(12) 0.0206(4) Uani 1 1 d .
H14A H 0.4119 1.0419 0.6890 0.031 Uiso 1 1 calc R
H14B H 0.4586 0.9627 0.6279 0.031 Uiso 1 1 calc R
H14C H 0.5232 1.0527 0.6686 0.031 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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
N1 W1 Cl1 91.708(11) . .
N1 W1 Cl1 91.707(11) . 2_656
Cl1 W1 Cl1 176.58(2) . 2_656
N1 W1 Cl2 180.0 . .
Cl1 W1 Cl2 88.292(11) . .
Cl1 W1 Cl2 88.293(11) 2_656 .
N1 W1 P1 95.623(11) . .
Cl1 W1 P1 92.671(16) . .
Cl1 W1 P1 86.994(16) 2_656 .
Cl2 W1 P1 84.377(11) . .
N1 W1 P1 95.622(11) . 2_656
Cl1 W1 P1 86.993(16) . 2_656
Cl1 W1 P1 92.672(16) 2_656 2_656
Cl2 W1 P1 84.378(11) . 2_656
P1 W1 P1 168.76(2) . 2_656
C1 P1 C13 105.10(9) . .
C1 P1 C7 106.11(9) . .
C13 P1 C7 101.53(9) . .
C1 P1 W1 117.49(7) . .
C13 P1 W1 110.95(7) . .
C7 P1 W1 114.11(6) . .
C14 N1 C14 108.9(2) 2_656 .
C14 N1 W1 125.57(10) 2_656 .
C14 N1 W1 125.57(10) . .
C6 C1 C2 118.52(18) . .
C6 C1 P1 121.51(16) . .
C2 C1 P1 119.94(14) . .
C3 C2 C1 120.51(19) . .
C3 C2 H2 119.7 . .
C1 C2 H2 119.7 . .
C2 C3 C4 120.3(2) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C5 C4 C3 119.7(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 120.2(2) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C5 C6 C1 120.7(2) . .
C5 C6 H6 119.6 . .
C1 C6 H6 119.6 . .
C8 C7 C12 118.98(18) . .
C8 C7 P1 123.53(15) . .
C12 C7 P1 117.45(15) . .
C7 C8 C9 120.27(18) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
C10 C9 C8 120.49(19) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C11 119.64(19) . .
C9 C10 H10 120.2 . .
C11 C10 H10 120.2 . .
C12 C11 C10 120.32(19) . .
C12 C11 H11 119.8 . .
C10 C11 H11 119.8 . .
C11 C12 C7 120.30(19) . .
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 . .
N1 C14 H14A 109.5 . .
N1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N1 1.928(2) .
W1 Cl1 2.3953(4) .
W1 Cl1 2.3953(4) 2_656
W1 Cl2 2.4500(6) .
W1 P1 2.5638(5) .
W1 P1 2.5638(5) 2_656
P1 C1 1.820(2) .
P1 C13 1.820(2) .
P1 C7 1.828(2) .
N1 C14 1.470(2) 2_656
N1 C14 1.470(2) .
C1 C6 1.394(3) .
C1 C2 1.400(3) .
C2 C3 1.385(3) .
C2 H2 0.9500 .
C3 C4 1.386(3) .
C3 H3 0.9500 .
C4 C5 1.385(3) .
C4 H4 0.9500 .
C5 C6 1.388(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.390(3) .
C7 C12 1.405(3) .
C8 C9 1.391(3) .
C8 H8 0.9500 .
C9 C10 1.384(3) .
C9 H9 0.9500 .
C10 C11 1.389(3) .
C10 H10 0.9500 .
C11 C12 1.384(3) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
