#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:46:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179863 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/59/7015948.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_7015948
loop_
_publ_author_name
'Benjamin, Sophie L.'
'Levason, William'
'Reid, Gillian'
'Rogers, Michael C.'
_publ_section_title
;
 Hybrid dibismuthines and distibines as ligands towards transition
 metal carbonyls.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6565
_journal_page_last               6574
_journal_paper_doi               10.1039/c1dt10447k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C21 H24 Cr O3 S Sb2'
_chemical_formula_structural     '(C18 H24 S Sb2) Cr (C O)3'
_chemical_formula_sum            'C21 H24 Cr O3 S Sb2'
_chemical_formula_weight         651.96
_chemical_name_systematic
;
Tricarbonyl(bis[(2-dimethylstibino)benzyl]sulfide)chromium(0)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-09-26
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record             '2010-12-15 Revised numbering scheme (mw)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.357(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6781(10)
_cell_length_b                   11.2606(10)
_cell_length_c                   16.5520(15)
_cell_measurement_reflns_used    23271
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2363.0(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29464
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+7.1018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                4746
_reflns_number_total             5404
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c1dt10447k.txt
_cod_data_source_block           10slbfaccr
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7015948
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.28764(4) 0.12582(5) 0.79887(3) 0.01925(12) Uani 1 1 d . . .
Sb1 Sb 0.315430(18) 0.23729(2) 0.663225(14) 0.01941(7) Uani 1 1 d . . .
Sb2 Sb 0.106127(18) 0.03685(2) 0.757348(15) 0.02182(7) Uani 1 1 d . . .
S1 S 0.37245(7) -0.04540(8) 0.74067(5) 0.02001(18) Uani 1 1 d . . .
O1 O 0.2681(3) 0.0074(3) 0.96016(17) 0.0430(8) Uani 1 1 d . . .
O2 O 0.1991(2) 0.3538(3) 0.86330(18) 0.0361(7) Uani 1 1 d . . .
O3 O 0.5014(2) 0.1976(3) 0.85955(19) 0.0389(7) Uani 1 1 d . . .
C1 C 0.3377(3) 0.4247(3) 0.6657(3) 0.0315(9) Uani 1 1 d . . .
H1A H 0.2750 0.4628 0.6884 0.047 Uiso 1 1 calc R . .
H1B H 0.3490 0.4538 0.6106 0.047 Uiso 1 1 calc R . .
H1C H 0.3993 0.4438 0.6993 0.047 Uiso 1 1 calc R . .
C2 C 0.2121(3) 0.2263(4) 0.5609(2) 0.0337(9) Uani 1 1 d . . .
H2A H 0.1412 0.2518 0.5764 0.051 Uiso 1 1 calc R . .
H2B H 0.2095 0.1441 0.5415 0.051 Uiso 1 1 calc R . .
H2C H 0.2384 0.2779 0.5178 0.051 Uiso 1 1 calc R . .
C3 C 0.4602(3) 0.1776(3) 0.6125(2) 0.0225(8) Uani 1 1 d . . .
C4 C 0.5394(3) 0.2561(4) 0.5898(2) 0.0256(8) Uani 1 1 d . . .
H4 H 0.5258 0.3391 0.5892 0.031 Uiso 1 1 calc R . .
C5 C 0.6377(3) 0.2144(4) 0.5680(2) 0.0292(9) Uani 1 1 d . . .
H5 H 0.6906 0.2687 0.5514 0.035 Uiso 1 1 calc R . .
C6 C 0.6594(3) 0.0945(4) 0.5702(2) 0.0292(9) Uani 1 1 d . . .
H6 H 0.7278 0.0666 0.5568 0.035 Uiso 1 1 calc R . .
C7 C 0.5813(3) 0.0144(4) 0.5920(2) 0.0256(8) Uani 1 1 d . . .
H7 H 0.5961 -0.0683 0.5928 0.031 Uiso 1 1 calc R . .
C8 C 0.4809(3) 0.0552(3) 0.6127(2) 0.0210(7) Uani 1 1 d . . .
C9 C 0.3955(3) -0.0341(3) 0.6317(2) 0.0209(7) Uani 1 1 d . . .
H9A H 0.4163 -0.1129 0.6106 0.025 Uiso 1 1 calc R . .
H9B H 0.3293 -0.0102 0.6043 0.025 Uiso 1 1 calc R . .
C10 C 0.2873(3) -0.1781(3) 0.7407(2) 0.0232(8) Uani 1 1 d . . .
H10A H 0.3329 -0.2492 0.7362 0.028 Uiso 1 1 calc R . .
H10B H 0.2512 -0.1824 0.7935 0.028 Uiso 1 1 calc R . .
C11 C 0.2050(3) -0.1842(3) 0.6752(2) 0.0216(7) Uani 1 1 d . . .
C12 C 0.2135(3) -0.2735(3) 0.6174(2) 0.0251(8) Uani 1 1 d . . .
H12 H 0.2722 -0.3258 0.6188 0.030 Uiso 1 1 calc R . .
C13 C 0.1373(3) -0.2868(4) 0.5581(2) 0.0324(9) Uani 1 1 d . . .
H13 H 0.1424 -0.3501 0.5204 0.039 Uiso 1 1 calc R . .
C14 C 0.0540(3) -0.2088(4) 0.5535(3) 0.0345(10) Uani 1 1 d . . .
H14 H 0.0023 -0.2175 0.5121 0.041 Uiso 1 1 calc R . .
C15 C 0.0457(3) -0.1175(4) 0.6092(2) 0.0298(9) Uani 1 1 d . . .
H15 H -0.0112 -0.0629 0.6050 0.036 Uiso 1 1 calc R . .
C16 C 0.1197(3) -0.1044(3) 0.6714(2) 0.0208(7) Uani 1 1 d . . .
C17 C 0.0181(3) -0.0532(4) 0.8491(3) 0.0364(10) Uani 1 1 d . . .
H17A H 0.0051 0.0013 0.8941 0.055 Uiso 1 1 calc R . .
H17B H 0.0585 -0.1218 0.8686 0.055 Uiso 1 1 calc R . .
H17C H -0.0494 -0.0802 0.8265 0.055 Uiso 1 1 calc R . .
C18 C -0.0246(3) 0.1286(4) 0.7057(3) 0.0372(10) Uani 1 1 d . . .
H18A H -0.0415 0.1979 0.7390 0.056 Uiso 1 1 calc R . .
H18B H -0.0858 0.0754 0.7034 0.056 Uiso 1 1 calc R . .
H18C H -0.0068 0.1546 0.6510 0.056 Uiso 1 1 calc R . .
C19 C 0.2740(3) 0.0506(3) 0.8971(2) 0.0268(8) Uani 1 1 d . . .
C20 C 0.2304(3) 0.2637(3) 0.8387(2) 0.0245(8) Uani 1 1 d . . .
C21 C 0.4193(3) 0.1720(3) 0.8332(2) 0.0245(8) Uani 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_publ_flag
C21 Cr1 C20 90.54(16) . . ?
C21 Cr1 C19 86.95(17) . . ?
C20 Cr1 C19 91.86(17) . . ?
C21 Cr1 S1 86.77(12) . . ?
C20 Cr1 S1 175.42(12) . . ?
C19 Cr1 S1 91.69(12) . . ?
C21 Cr1 Sb1 90.16(12) . . ?
C20 Cr1 Sb1 87.58(12) . . ?
C19 Cr1 Sb1 177.05(12) . . ?
S1 Cr1 Sb1 88.73(3) . . ?
C21 Cr1 Sb2 173.46(12) . . ?
C20 Cr1 Sb2 94.01(11) . . ?
C19 Cr1 Sb2 88.20(12) . . ?
S1 Cr1 Sb2 88.99(3) . . ?
Sb1 Cr1 Sb2 94.72(2) . . ?
C1 Sb1 C3 101.86(15) . . ?
C1 Sb1 C2 98.81(16) . . ?
C3 Sb1 C2 101.21(15) . . ?
C1 Sb1 Cr1 118.73(12) . . ?
C3 Sb1 Cr1 108.04(10) . . ?
C2 Sb1 Cr1 124.82(12) . . ?
C18 Sb2 C16 99.18(16) . . ?
C18 Sb2 C17 96.12(18) . . ?
C16 Sb2 C17 99.41(15) . . ?
C18 Sb2 Cr1 127.26(12) . . ?
C16 Sb2 Cr1 112.79(9) . . ?
C17 Sb2 Cr1 117.30(13) . . ?
C9 S1 C10 98.82(16) . . ?
C9 S1 Cr1 114.32(12) . . ?
C10 S1 Cr1 112.68(13) . . ?
Sb1 C1 H1A 109.5 . . ?
Sb1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sb1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sb1 C2 H2A 109.5 . . ?
Sb1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sb1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.3(3) . . ?
C4 C3 Sb1 122.1(3) . . ?
C8 C3 Sb1 118.1(3) . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.0(4) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 120.1(4) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C7 C8 C3 119.6(3) . . ?
C7 C8 C9 119.1(3) . . ?
C3 C8 C9 121.3(3) . . ?
C8 C9 S1 111.7(2) . . ?
C8 C9 H9A 109.3 . . ?
S1 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
S1 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 S1 116.2(2) . . ?
C11 C10 H10A 108.2 . . ?
S1 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
S1 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C12 C11 C16 119.6(3) . . ?
C12 C11 C10 118.2(3) . . ?
C16 C11 C10 122.2(3) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C16 121.0(4) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 118.5(3) . . ?
C15 C16 Sb2 120.8(3) . . ?
C11 C16 Sb2 120.7(3) . . ?
Sb2 C17 H17A 109.5 . . ?
Sb2 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Sb2 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Sb2 C18 H18A 109.5 . . ?
Sb2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Sb2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 C19 Cr1 177.0(3) . . ?
O2 C20 Cr1 176.6(3) . . ?
O3 C21 Cr1 175.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 C21 1.835(4) . ?
Cr1 C20 1.838(4) . ?
Cr1 C19 1.842(4) . ?
Cr1 S1 2.4114(11) . ?
Cr1 Sb1 2.5982(6) . ?
Cr1 Sb2 2.5985(6) . ?
Sb1 C1 2.129(4) . ?
Sb1 C3 2.131(4) . ?
Sb1 C2 2.139(4) . ?
Sb2 C18 2.128(4) . ?
Sb2 C16 2.141(4) . ?
Sb2 C17 2.145(4) . ?
S1 C9 1.833(4) . ?
S1 C10 1.844(4) . ?
O1 C19 1.155(5) . ?
O2 C20 1.164(5) . ?
O3 C21 1.162(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.391(5) . ?
C3 C8 1.403(5) . ?
C4 C5 1.382(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.398(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.512(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.501(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.392(5) . ?
C11 C16 1.407(5) . ?
C12 C13 1.381(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.374(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.397(5) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
