#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/39/4073965.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_4073965
loop_
_publ_author_name
'Darensbourg, Donald J.'
'Andreatta, Jeremy R.'
'Stranahan, Sarah M.'
'Reibenspies, Joseph H.'
_publ_section_title
;
 What is the Real Steric Impact of Triphenylphosphite? Solid-State and
 Solution Structural Studies ofcis- andtrans-Isomers of M(CO)4[P(OPh)3]2(M
 = Mo and W)
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6832
_journal_paper_doi               10.1021/om700761q
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C20.5 H15.5 Cl1.5 O5 P W0.5'
_chemical_formula_weight         517.90
_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                69.75
_cell_angle_beta                 89.76
_cell_angle_gamma                68.30
_cell_formula_units_Z            2
_cell_length_a                   9.170
_cell_length_b                   11.151
_cell_length_c                   11.375
_cell_measurement_reflns_used    3453
_cell_measurement_temperature    110(2)
_cell_volume                     1003.645
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7889
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  0.7393
_exptl_absorpt_correction_T_min  0.5657
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0200
_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)+(0.0253P)²+0.6716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0490
_reflns_number_gt                3449
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700761q-file008.cif
_cod_data_source_block           jer
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1003.7
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C20.50 H15.50 Cl1.50 O5 P W0.50'
_cod_database_code               4073965
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9973(3) -0.1401(3) 0.9242(2) 0.0205(6) Uani 1 1 d . . .
C2 C 1.1765(3) 0.0247(3) 0.8958(3) 0.0218(6) Uani 1 1 d . . .
C3 C 0.9599(3) 0.3576(3) 0.7283(2) 0.0199(6) Uani 1 1 d . . .
C4 C 1.0781(4) 0.3672(3) 0.6540(3) 0.0270(6) Uani 1 1 d . . .
H4 H 1.1026 0.3203 0.5964 0.032 Uiso 1 1 calc R . .
C5 C 1.1602(4) 0.4464(4) 0.6648(3) 0.0360(8) Uani 1 1 d . . .
H5 H 1.2414 0.4538 0.6141 0.043 Uiso 1 1 calc R . .
C6 C 1.1246(4) 0.5144(3) 0.7488(3) 0.0344(7) Uani 1 1 d . . .
H6 H 1.1814 0.5681 0.7560 0.041 Uiso 1 1 calc R . .
C7 C 1.0066(4) 0.5042(3) 0.8220(3) 0.0285(6) Uani 1 1 d . . .
H7 H 0.9820 0.5514 0.8794 0.034 Uiso 1 1 calc R . .
C8 C 0.9231(3) 0.4252(3) 0.8127(3) 0.0233(6) Uani 1 1 d . . .
H8 H 0.8420 0.4178 0.8635 0.028 Uiso 1 1 calc R . .
C9 C 0.5672(3) 0.2770(3) 0.9274(3) 0.0199(6) Uani 1 1 d . . .
C10 C 0.5791(4) 0.3244(3) 1.0223(3) 0.0274(6) Uani 1 1 d . . .
H10 H 0.6518 0.3666 1.0235 0.033 Uiso 1 1 calc R . .
C11 C 0.4824(4) 0.3095(3) 1.1165(3) 0.0314(7) Uani 1 1 d . . .
H11 H 0.4880 0.3426 1.1822 0.038 Uiso 1 1 calc R . .
C12 C 0.3784(4) 0.2465(3) 1.1146(3) 0.0292(7) Uani 1 1 d . . .
H12 H 0.3121 0.2369 1.1787 0.035 Uiso 1 1 calc R . .
C13 C 0.3705(4) 0.1975(3) 1.0193(3) 0.0314(7) Uani 1 1 d . . .
H13 H 0.2998 0.1531 1.0190 0.038 Uiso 1 1 calc R . .
C14 C 0.4653(3) 0.2128(3) 0.9242(3) 0.0260(6) Uani 1 1 d . . .
H14 H 0.4601 0.1797 0.8585 0.031 Uiso 1 1 calc R . .
C15 C 0.6282(3) 0.1819(3) 0.6322(2) 0.0186(5) Uani 1 1 d . . .
C16 C 0.5343(3) 0.1094(3) 0.6323(3) 0.0257(6) Uani 1 1 d . . .
H16 H 0.5534 0.0232 0.6991 0.031 Uiso 1 1 calc R . .
C17 C 0.4115(4) 0.1642(3) 0.5337(3) 0.0295(7) Uani 1 1 d . . .
H17 H 0.3472 0.1146 0.5322 0.035 Uiso 1 1 calc R . .
C18 C 0.3824(4) 0.2907(3) 0.4374(3) 0.0298(7) Uani 1 1 d . . .
H18 H 0.2972 0.3286 0.3708 0.036 Uiso 1 1 calc R . .
C19 C 0.4778(4) 0.3615(3) 0.4387(3) 0.0303(7) Uani 1 1 d . . .
H19 H 0.4583 0.4480 0.3723 0.036 Uiso 1 1 calc R . .
C20 C 0.6022(4) 0.3076(3) 0.5363(3) 0.0266(6) Uani 1 1 d . . .
H20 H 0.6680 0.3562 0.5369 0.032 Uiso 1 1 calc R . .
C1S C 0.0170(5) 0.9948(4) 0.5532(4) 0.0346(15) Uani 0.50 1 d PD A -1
H1SA H -0.0347 1.0055 0.6246 0.042 Uiso 0.50 1 d PR A -1
Cl1 Cl 0.20711(19) 0.89727(17) 0.64452(15) 0.0369(4) Uani 0.50 1 d PD A -1
Cl2 Cl -0.0304(3) 0.8950(3) 0.4794(3) 0.0599(6) Uani 0.50 1 d PD A -1
Cl3 Cl 0.0125(3) 1.1512(2) 0.4379(2) 0.0526(5) Uani 0.50 1 d PD A -1
O1 O 0.9961(3) -0.2165(2) 0.87855(19) 0.0287(5) Uani 1 1 d . . .
O2 O 1.2706(2) 0.0414(2) 0.8333(2) 0.0297(5) Uani 1 1 d . . .
O3 O 0.8784(2) 0.28052(19) 0.70868(17) 0.0196(4) Uani 1 1 d . . .
O4 O 0.6589(2) 0.30065(19) 0.82874(17) 0.0204(4) Uani 1 1 d . . .
O5 O 0.7530(2) 0.11627(19) 0.73269(17) 0.0204(4) Uani 1 1 d . . .
P1 P 0.81770(8) 0.17918(7) 0.81803(6) 0.01632(14) Uani 1 1 d . . .
W1 W 1.0000 0.0000 1.0000 0.02121(7) Uani 1 2 d S . .
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'
O O 0.0106 0.0060 '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
O1 C1 W1 178.2(2) . .
O2 C2 W1 177.2(2) . .
C8 C3 C4 121.0(3) . .
C8 C3 O3 123.2(2) . .
C4 C3 O3 115.8(2) . .
C3 C4 C5 119.1(3) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C6 C5 C4 120.4(3) . .
C6 C5 H5 119.8 . .
C4 C5 H5 119.8 . .
C7 C6 C5 119.9(3) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C6 C7 C8 120.5(3) . .
C6 C7 H7 119.7 . .
C8 C7 H7 119.7 . .
C3 C8 C7 119.0(3) . .
C3 C8 H8 120.5 . .
C7 C8 H8 120.5 . .
C10 C9 C14 122.1(3) . .
C10 C9 O4 117.9(2) . .
C14 C9 O4 119.9(2) . .
C9 C10 C11 118.8(3) . .
C9 C10 H10 120.6 . .
C11 C10 H10 120.6 . .
C12 C11 C10 120.1(3) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.1(3) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C12 C13 C14 120.4(3) . .
C12 C13 H13 119.8 . .
C14 C13 H13 119.8 . .
C9 C14 C13 118.6(3) . .
C9 C14 H14 120.7 . .
C13 C14 H14 120.7 . .
C20 C15 C16 121.4(3) . .
C20 C15 O5 123.3(2) . .
C16 C15 O5 115.2(2) . .
C15 C16 C17 119.1(3) . .
C15 C16 H16 120.4 . .
C17 C16 H16 120.4 . .
C18 C17 C16 120.4(3) . .
C18 C17 H17 119.8 . .
C16 C17 H17 119.8 . .
C19 C18 C17 119.7(3) . .
C19 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C18 C19 C20 120.7(3) . .
C18 C19 H19 119.6 . .
C20 C19 H19 119.6 . .
C15 C20 C19 118.7(3) . .
C15 C20 H20 120.7 . .
C19 C20 H20 120.7 . .
Cl3 C1S Cl1 110.2(2) . .
Cl3 C1S Cl2 110.3(3) . .
Cl1 C1S Cl2 109.6(3) . .
Cl3 C1S H1SA 114.6 . .
Cl1 C1S H1SA 93.5 . .
Cl2 C1S H1SA 117.3 . .
C3 O3 P1 125.42(16) . .
C9 O4 P1 122.66(16) . .
C15 O5 P1 130.21(17) . .
O5 P1 O3 98.53(10) . .
O5 P1 O4 103.43(10) . .
O3 P1 O4 96.32(10) . .
O5 P1 W1 111.93(7) . .
O3 P1 W1 120.08(7) . .
O4 P1 W1 122.69(7) . .
C1 W1 C1 180.0 2_757 .
C1 W1 C2 92.29(10) 2_757 .
C1 W1 C2 87.71(10) . .
C1 W1 C2 87.71(10) 2_757 2_757
C1 W1 C2 92.29(10) . 2_757
C2 W1 C2 180.0 . 2_757
C1 W1 P1 92.14(8) 2_757 .
C1 W1 P1 87.86(8) . .
C2 W1 P1 86.50(8) . .
C2 W1 P1 93.50(8) 2_757 .
C1 W1 P1 87.87(8) 2_757 2_757
C1 W1 P1 92.14(8) . 2_757
C2 W1 P1 93.50(8) . 2_757
C2 W1 P1 86.50(8) 2_757 2_757
P1 W1 P1 180.0 . 2_757
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.144(3) .
C1 W1 2.036(3) .
C2 O2 1.143(3) .
C2 W1 2.047(3) .
C3 C8 1.383(4) .
C3 C4 1.384(4) .
C3 O3 1.398(3) .
C4 C5 1.389(4) .
C4 H4 0.9500 .
C5 C6 1.383(5) .
C5 H5 0.9500 .
C6 C7 1.376(4) .
C6 H6 0.9500 .
C7 C8 1.392(4) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.377(4) .
C9 C14 1.378(4) .
C9 O4 1.409(3) .
C10 C11 1.393(4) .
C10 H10 0.9500 .
C11 C12 1.382(4) .
C11 H11 0.9500 .
C12 C13 1.385(4) .
C12 H12 0.9500 .
C13 C14 1.390(4) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C15 C20 1.381(4) .
C15 C16 1.382(4) .
C15 O5 1.402(3) .
C16 C17 1.388(4) .
C16 H16 0.9500 .
C17 C18 1.384(4) .
C17 H17 0.9500 .
C18 C19 1.382(4) .
C18 H18 0.9500 .
C19 C20 1.391(4) .
C19 H19 0.9500 .
C20 H20 0.9500 .
C1S Cl3 1.769(4) .
C1S Cl1 1.770(4) .
C1S Cl2 1.772(4) .
C1S H1SA 0.9600 .
O3 P1 1.6190(18) .
O4 P1 1.6197(19) .
O5 P1 1.6034(18) .
P1 W1 2.4017(7) .
W1 C1 2.036(3) 2_757
W1 C2 2.047(3) 2_757
W1 P1 2.4017(7) 2_757
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
_geom_torsion_site_symmetry_4
C8 C3 C4 C5 -0.1(4) .
O3 C3 C4 C5 177.6(3) .
C3 C4 C5 C6 0.1(5) .
C4 C5 C6 C7 -0.2(5) .
C5 C6 C7 C8 0.3(5) .
C4 C3 C8 C7 0.2(4) .
O3 C3 C8 C7 -177.4(3) .
C6 C7 C8 C3 -0.3(4) .
C14 C9 C10 C11 -1.4(4) .
O4 C9 C10 C11 176.2(3) .
C9 C10 C11 C12 0.8(5) .
C10 C11 C12 C13 0.3(5) .
C11 C12 C13 C14 -0.9(5) .
C10 C9 C14 C13 0.9(4) .
O4 C9 C14 C13 -176.7(3) .
C12 C13 C14 C9 0.3(5) .
C20 C15 C16 C17 0.2(4) .
O5 C15 C16 C17 -177.6(2) .
C15 C16 C17 C18 -0.9(4) .
C16 C17 C18 C19 1.1(5) .
C17 C18 C19 C20 -0.5(5) .
C16 C15 C20 C19 0.4(4) .
O5 C15 C20 C19 178.0(2) .
C18 C19 C20 C15 -0.2(5) .
C8 C3 O3 P1 -40.0(4) .
C4 C3 O3 P1 142.4(2) .
C10 C9 O4 P1 104.6(3) .
C14 C9 O4 P1 -77.8(3) .
C20 C15 O5 P1 44.0(4) .
C16 C15 O5 P1 -138.3(2) .
C15 O5 P1 O3 -64.3(2) .
C15 O5 P1 O4 34.3(2) .
C15 O5 P1 W1 168.35(19) .
C3 O3 P1 O5 -174.8(2) .
C3 O3 P1 O4 80.6(2) .
C3 O3 P1 W1 -53.2(2) .
C9 O4 P1 O5 90.9(2) .
C9 O4 P1 O3 -168.75(19) .
C9 O4 P1 W1 -36.7(2) .
O1 C1 W1 C1 13(8) 2_757
O1 C1 W1 C2 -43(8) .
O1 C1 W1 C2 137(8) 2_757
O1 C1 W1 P1 44(8) .
O1 C1 W1 P1 -136(8) 2_757
O2 C2 W1 C1 -107(5) 2_757
O2 C2 W1 C1 73(5) .
O2 C2 W1 C2 43(5) 2_757
O2 C2 W1 P1 -15(5) .
O2 C2 W1 P1 165(5) 2_757
O5 P1 W1 C1 -170.89(11) 2_757
O3 P1 W1 C1 74.40(11) 2_757
O4 P1 W1 C1 -47.12(11) 2_757
O5 P1 W1 C1 9.11(11) .
O3 P1 W1 C1 -105.60(11) .
O4 P1 W1 C1 132.88(11) .
O5 P1 W1 C2 96.95(11) .
O3 P1 W1 C2 -17.76(11) .
O4 P1 W1 C2 -139.28(11) .
O5 P1 W1 C2 -83.05(11) 2_757
O3 P1 W1 C2 162.24(11) 2_757
O4 P1 W1 C2 40.72(11) 2_757
O5 P1 W1 P1 -19.05(10) 2_757
O3 P1 W1 P1 -133.76(14) 2_757
O4 P1 W1 P1 104.72(12) 2_757
