#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:34:13 +0100 (lun 21 de mar de 2016) $
#$Revision: 178571 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/81/4068117.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_4068117
loop_
_publ_author_name
'Benjamin, Sophie L.'
'Levason, William'
'Reid, Gillian'
'Warr, Robert P.'
_publ_section_title
;
 Halostibines SbMeX2and SbMe2X: Lewis Acids or Lewis Bases?
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              1025
_journal_paper_doi               10.1021/om2010996
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C7 H6 Br Cr O5 Sb'
_chemical_formula_structural     '(C2 H6 Br Sb) (C O)5 Cr'
_chemical_formula_sum            'C7 H6 Br Cr O5 Sb'
_chemical_formula_weight         423.78
_chemical_name_systematic
;
 pentacarbonyl(bromo(dimethyl)stibine)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             2011-04-28
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record             '2011-09-30 Added Sb1...O2 contact'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.735(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.261(5)
_cell_length_b                   6.488(5)
_cell_length_c                   12.287(5)
_cell_measurement_reflns_used    50128
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1234.7(11)
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14744
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.300
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.208
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0897P)²+13.0506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                2289
_reflns_number_total             2377
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om2010996_si_002.cif
_cod_data_source_block           11slb121
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068117
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
Cr1 Cr 0.33942(8) -0.00312(19) 0.31635(10) 0.0171(3) Uani 1 1 d .
Sb1 Sb 0.18932(3) 0.10384(9) 0.32571(4) 0.0229(3) Uani 1 1 d .
Br1 Br 0.07917(7) 0.0168(3) 0.13709(9) 0.0620(5) Uani 1 1 d .
O1 O 0.2712(5) -0.4057(10) 0.2011(6) 0.0335(16) Uani 1 1 d .
O2 O 0.2964(4) 0.1918(10) 0.0805(5) 0.0306(14) Uani 1 1 d .
O3 O 0.4193(5) 0.4029(10) 0.4247(6) 0.0342(16) Uani 1 1 d .
O4 O 0.3789(5) -0.2159(11) 0.5475(5) 0.0347(15) Uani 1 1 d .
O5 O 0.5140(4) -0.1340(11) 0.3018(6) 0.0349(15) Uani 1 1 d .
C1 C 0.1226(7) -0.0379(16) 0.4302(8) 0.034(2) Uani 1 1 d .
H1A H 0.1343 -0.1863 0.4348 0.050 Uiso 1 1 calc R
H1B H 0.0604 -0.0146 0.3970 0.050 Uiso 1 1 calc R
H1C H 0.1423 0.0220 0.5071 0.050 Uiso 1 1 calc R
C2 C 0.1487(8) 0.4165(17) 0.3349(12) 0.047(3) Uani 1 1 d .
H2A H 0.1747 0.5053 0.2898 0.070 Uiso 1 1 calc R
H2B H 0.1673 0.4623 0.4147 0.070 Uiso 1 1 calc R
H2C H 0.0857 0.4246 0.3045 0.070 Uiso 1 1 calc R
C3 C 0.2940(6) -0.2527(14) 0.2449(7) 0.0241(17) Uani 1 1 d .
C4 C 0.3126(6) 0.1213(13) 0.1698(7) 0.0233(18) Uani 1 1 d .
C5 C 0.3881(5) 0.2503(13) 0.3851(6) 0.0217(16) Uani 1 1 d .
C6 C 0.3636(6) -0.1348(14) 0.4613(7) 0.0237(17) Uani 1 1 d .
C7 C 0.4471(6) -0.0824(13) 0.3065(7) 0.0218(17) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0172(6) 0.0220(7) 0.0114(6) -0.0016(5) 0.0032(5) -0.0006(5)
Sb1 0.0187(4) 0.0323(4) 0.0169(4) 0.0009(2) 0.0042(2) 0.0014(2)
Br1 0.0236(6) 0.1338(14) 0.0225(5) -0.0126(6) -0.0018(4) -0.0053(6)
O1 0.040(4) 0.030(4) 0.030(4) -0.007(3) 0.009(3) -0.010(3)
O2 0.040(4) 0.033(3) 0.018(3) 0.005(3) 0.008(3) 0.003(3)
O3 0.032(4) 0.033(4) 0.032(4) -0.011(3) 0.003(3) -0.007(3)
O4 0.047(4) 0.038(4) 0.021(3) 0.007(3) 0.012(3) 0.010(3)
O5 0.025(3) 0.042(4) 0.039(4) -0.009(3) 0.013(3) 0.004(3)
C1 0.038(5) 0.039(5) 0.029(5) 0.001(4) 0.016(4) -0.004(4)
C2 0.043(6) 0.044(6) 0.066(8) 0.028(5) 0.034(6) 0.025(5)
C3 0.029(4) 0.028(4) 0.015(4) 0.000(3) 0.006(3) -0.002(3)
C4 0.027(5) 0.022(4) 0.021(4) -0.005(3) 0.008(4) -0.005(3)
C5 0.021(4) 0.027(4) 0.016(4) -0.001(3) 0.003(3) 0.005(3)
C6 0.026(4) 0.027(4) 0.018(4) -0.003(3) 0.006(3) -0.004(3)
C7 0.028(4) 0.023(4) 0.013(4) -0.003(3) 0.004(3) 0.004(3)
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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C7 Cr1 C3 88.6(4)
C7 Cr1 C4 90.3(4)
C3 Cr1 C4 88.8(4)
C7 Cr1 C6 90.4(4)
C3 Cr1 C6 89.4(4)
C4 Cr1 C6 178.1(4)
C7 Cr1 C5 89.7(4)
C3 Cr1 C5 177.9(4)
C4 Cr1 C5 89.9(3)
C6 Cr1 C5 91.9(4)
C7 Cr1 Sb1 178.8(3)
C3 Cr1 Sb1 90.6(3)
C4 Cr1 Sb1 88.9(3)
C6 Cr1 Sb1 90.4(3)
C5 Cr1 Sb1 91.1(2)
C1 Sb1 C2 98.9(4)
C1 Sb1 Br1 96.2(3)
C2 Sb1 Br1 96.7(4)
C1 Sb1 Cr1 125.2(3)
C2 Sb1 Cr1 124.6(3)
Br1 Sb1 Cr1 108.42(5)
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
O1 C3 Cr1 176.0(8)
O2 C4 Cr1 178.4(7)
O3 C5 Cr1 177.8(8)
O4 C6 Cr1 178.8(8)
O5 C7 Cr1 178.9(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cr1 C7 1.864(9)
Cr1 C3 1.882(9)
Cr1 C4 1.899(9)
Cr1 C6 1.905(9)
Cr1 C5 1.907(9)
Cr1 Sb1 2.5736(15)
Sb1 C1 2.126(9)
Sb1 C2 2.147(11)
Sb1 Br1 2.5239(13)
O1 C3 1.136(11)
O2 C4 1.143(11)
O3 C5 1.151(11)
O4 C6 1.140(11)
O5 C7 1.156(11)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Sb1 O2 3.357(6) 4_566
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
Br1 Sb1 Cr1 C3 -43.2(3)
Br1 Sb1 Cr1 C4 45.6(3)
