#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:16:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179782 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/78/7007816.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_7007816
loop_
_publ_author_name
'Brown, Michael D.'
'Levason, William'
'Reid, Gillian'
'Webster, Michael'
_publ_section_title
;
 Preparation and coordinating properties of {CH2(o-C6H4CH2SbMe2)}2, a
 novel wide-angle cis-chelating distibine.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5648
_journal_page_last               5654
_journal_paper_doi               10.1039/b610808c
_journal_year                    2006
_chemical_formula_moiety         'C24 H28 O4 Sb2 W'
_chemical_formula_sum            'C24 H28 O4 Sb2 W'
_chemical_formula_weight         807.81
_chemical_name_common
;tetracarbonyl(1,2-bis((2-
dimethylstibinomethyl)phenyl)ethane)tungsten(0)
;
_chemical_name_systematic
;
tetracarbonyl(1,2-bis((2-dimethylstibinomethyl)phenyl)ethane)tungsten(0)
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-07-18
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.506(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.705(3)
_cell_length_b                   11.6869(15)
_cell_length_c                   12.4991(10)
_cell_measurement_reflns_used    2908
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2578.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17199
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.557
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.031
_refine_diff_density_min         -1.338
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.208(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5633
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0235
_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)+(0.0198P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                5428
_reflns_number_total             5633
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b610808c.txt
_cod_data_source_block           06mdb003
_cod_original_cell_volume        2578.2(5)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7007816
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'
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
W1 W 0.980999(11) 0.961247(14) 0.552447(13) 0.01959(5) Uani 1 1 d . . .
Sb1 Sb 0.874861(17) 0.78825(3) 0.55926(2) 0.02388(8) Uani 1 1 d . . .
Sb2 Sb 1.068267(18) 0.82487(3) 0.43084(2) 0.02490(8) Uani 1 1 d . . .
O1 O 1.0702(2) 0.8608(3) 0.7618(3) 0.0367(9) Uani 1 1 d . . .
O2 O 0.9006(2) 1.1051(3) 0.3597(3) 0.0345(8) Uani 1 1 d . . .
O3 O 0.8775(2) 1.0933(3) 0.7036(3) 0.0330(9) Uani 1 1 d . . .
O4 O 1.1059(3) 1.1531(4) 0.5545(4) 0.0488(11) Uani 1 1 d . . .
C1 C 0.7703(3) 0.8309(4) 0.6241(4) 0.0322(12) Uani 1 1 d . . .
H1A H 0.7805 0.8774 0.6889 0.048 Uiso 1 1 calc R . .
H1B H 0.7440 0.7606 0.6423 0.048 Uiso 1 1 calc R . .
H1C H 0.7384 0.8744 0.5708 0.048 Uiso 1 1 calc R . .
C2 C 0.8293(3) 0.6894(5) 0.4232(5) 0.0407(14) Uani 1 1 d . . .
H2A H 0.8709 0.6619 0.3827 0.061 Uiso 1 1 calc R . .
H2B H 0.7953 0.7376 0.3768 0.061 Uiso 1 1 calc R . .
H2C H 0.8010 0.6240 0.4484 0.061 Uiso 1 1 calc R . .
C3 C 0.9144(3) 0.6559(5) 0.6713(4) 0.0305(12) Uani 1 1 d . . .
H3A H 0.9699 0.6474 0.6684 0.037 Uiso 1 1 calc R . .
H3B H 0.9050 0.6809 0.7447 0.037 Uiso 1 1 calc R . .
C4 C 0.8777(3) 0.5406(4) 0.6508(5) 0.0281(13) Uani 1 1 d . . .
C5 C 0.8063(3) 0.5223(5) 0.6807(5) 0.0372(14) Uani 1 1 d . . .
H5 H 0.7812 0.5835 0.7132 0.045 Uiso 1 1 calc R . .
C6 C 0.7685(4) 0.4189(6) 0.6659(5) 0.0463(16) Uani 1 1 d . . .
H6 H 0.7180 0.4109 0.6854 0.056 Uiso 1 1 calc R . .
C7 C 0.8048(3) 0.3292(5) 0.6233(5) 0.0361(13) Uani 1 1 d . . .
H7 H 0.7808 0.2566 0.6158 0.043 Uiso 1 1 calc R . .
C8 C 0.8769(4) 0.3448(5) 0.5910(5) 0.0441(15) Uani 1 1 d . . .
H8 H 0.9004 0.2833 0.5566 0.053 Uiso 1 1 calc R . .
C9 C 0.9172(3) 0.4489(5) 0.6073(5) 0.0326(13) Uani 1 1 d . . .
C10 C 0.9996(3) 0.4541(5) 0.5737(5) 0.0358(14) Uani 1 1 d . . .
H10A H 1.0312 0.4989 0.6275 0.043 Uiso 1 1 calc R . .
H10B H 1.0206 0.3757 0.5724 0.043 Uiso 1 1 calc R . .
C11 C 1.0032(3) 0.5066(5) 0.4679(5) 0.0339(12) Uani 1 1 d . . .
H11A H 0.9882 0.5880 0.4715 0.041 Uiso 1 1 calc R . .
H11B H 0.9669 0.4677 0.4157 0.041 Uiso 1 1 calc R . .
C12 C 1.0819(3) 0.4985(5) 0.4299(4) 0.0280(11) Uani 1 1 d . . .
C13 C 1.1008(3) 0.4053(5) 0.3678(4) 0.0317(12) Uani 1 1 d . . .
H13 H 1.0639 0.3477 0.3516 0.038 Uiso 1 1 calc R . .
C14 C 1.1713(3) 0.3935(5) 0.3291(4) 0.0313(12) Uani 1 1 d . . .
H14 H 1.1824 0.3288 0.2872 0.038 Uiso 1 1 calc R . .
C15 C 1.2256(3) 0.4771(4) 0.3519(4) 0.0297(12) Uani 1 1 d . . .
H15 H 1.2741 0.4712 0.3246 0.036 Uiso 1 1 calc R . .
C16 C 1.2081(3) 0.5703(4) 0.4156(4) 0.0253(11) Uani 1 1 d . . .
H16 H 1.2454 0.6276 0.4311 0.030 Uiso 1 1 calc R . .
C17 C 1.1379(2) 0.5817(4) 0.4567(3) 0.0182(9) Uani 1 1 d . . .
C18 C 1.1204(3) 0.6838(4) 0.5223(4) 0.0228(10) Uani 1 1 d . . .
H18A H 1.1680 0.7113 0.5607 0.027 Uiso 1 1 calc R . .
H18B H 1.0861 0.6600 0.5771 0.027 Uiso 1 1 calc R . .
C19 C 1.0270(3) 0.7385(6) 0.2891(4) 0.0423(15) Uani 1 1 d . . .
H19A H 0.9793 0.6999 0.3013 0.064 Uiso 1 1 calc R . .
H19B H 1.0643 0.6816 0.2698 0.064 Uiso 1 1 calc R . .
H19C H 1.0183 0.7938 0.2305 0.064 Uiso 1 1 calc R . .
C20 C 1.1683(3) 0.8946(6) 0.3712(5) 0.0481(17) Uani 1 1 d . . .
H20A H 1.1960 0.9394 0.4278 0.072 Uiso 1 1 calc R . .
H20B H 1.1542 0.9442 0.3096 0.072 Uiso 1 1 calc R . .
H20C H 1.2006 0.8322 0.3489 0.072 Uiso 1 1 calc R . .
C21 C 1.0372(3) 0.8932(4) 0.6844(4) 0.0234(11) Uani 1 1 d . . .
C22 C 0.9284(3) 1.0470(4) 0.4253(5) 0.0272(12) Uani 1 1 d . . .
C23 C 0.9161(3) 1.0446(4) 0.6467(4) 0.0240(11) Uani 1 1 d . . .
C24 C 1.0590(3) 1.0813(5) 0.5540(4) 0.0316(12) 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'
Sb Sb -0.5866 1.5461 '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
_geom_angle_publ_flag
C23 W1 C24 94.8(2) . . ?
C23 W1 C21 88.8(2) . . ?
C24 W1 C21 88.4(2) . . ?
C23 W1 C22 88.3(2) . . ?
C24 W1 C22 86.3(2) . . ?
C21 W1 C22 173.7(2) . . ?
C23 W1 Sb2 174.31(13) . . ?
C24 W1 Sb2 89.66(15) . . ?
C21 W1 Sb2 87.78(14) . . ?
C22 W1 Sb2 95.50(15) . . ?
C23 W1 Sb1 85.04(14) . . ?
C24 W1 Sb1 177.23(16) . . ?
C21 W1 Sb1 88.80(13) . . ?
C22 W1 Sb1 96.50(15) . . ?
Sb2 W1 Sb1 90.339(14) . . ?
C1 Sb1 C2 98.2(2) . . ?
C1 Sb1 C3 99.6(2) . . ?
C2 Sb1 C3 102.1(2) . . ?
C1 Sb1 W1 116.86(14) . . ?
C2 Sb1 W1 125.41(17) . . ?
C3 Sb1 W1 110.85(14) . . ?
C19 Sb2 C20 97.5(3) . . ?
C19 Sb2 C18 100.5(2) . . ?
C20 Sb2 C18 98.3(2) . . ?
C19 Sb2 W1 124.41(16) . . ?
C20 Sb2 W1 119.18(18) . . ?
C18 Sb2 W1 112.45(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 Sb1 114.5(3) . . ?
C4 C3 H3A 108.6 . . ?
Sb1 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
Sb1 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C5 C4 C9 119.0(5) . . ?
C5 C4 C3 119.3(5) . . ?
C9 C4 C3 121.6(5) . . ?
C4 C5 C6 123.3(6) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C7 C6 C5 119.1(6) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 119.3(5) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C7 C8 C9 122.6(6) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C4 C9 C8 116.6(5) . . ?
C4 C9 C10 125.4(5) . . ?
C8 C9 C10 118.0(5) . . ?
C11 C10 C9 111.7(5) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 111.3(5) . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C17 118.5(5) . . ?
C13 C12 C11 119.5(5) . . ?
C17 C12 C11 122.1(5) . . ?
C14 C13 C12 122.4(5) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C16 119.0(5) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C17 C16 C15 122.1(5) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C12 118.6(5) . . ?
C16 C17 C18 120.7(4) . . ?
C12 C17 C18 120.6(4) . . ?
C17 C18 Sb2 114.5(3) . . ?
C17 C18 H18A 108.6 . . ?
Sb2 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
Sb2 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
Sb2 C19 H19A 109.5 . . ?
Sb2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Sb2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Sb2 C20 H20A 109.5 . . ?
Sb2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Sb2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O1 C21 W1 176.0(4) . . ?
O2 C22 W1 173.1(4) . . ?
O3 C23 W1 179.3(4) . . ?
O4 C24 W1 179.7(5) . . ?
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
W1 C23 1.966(5) . ?
W1 C24 1.968(5) . ?
W1 C21 2.021(5) . ?
W1 C22 2.041(6) . ?
W1 Sb2 2.7580(4) . ?
W1 Sb1 2.7661(4) . ?
Sb1 C1 2.138(5) . ?
Sb1 C2 2.159(5) . ?
Sb1 C3 2.165(5) . ?
Sb2 C19 2.119(6) . ?
Sb2 C20 2.136(5) . ?
Sb2 C18 2.171(5) . ?
O1 C21 1.155(6) . ?
O2 C22 1.146(6) . ?
O3 C23 1.173(6) . ?
O4 C24 1.179(6) . ?
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 1.509(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.363(8) . ?
C4 C9 1.412(8) . ?
C5 C6 1.387(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.360(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.381(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.417(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.551(8) . ?
C10 C11 1.463(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.511(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.394(8) . ?
C12 C17 1.410(7) . ?
C13 C14 1.379(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.494(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
