#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:34:13 +0100 (lun 21 de mar de 2016) $
#$Revision: 178571 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/81/4068119.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_4068119
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         'C6 H3 Br2 O5 Sb W'
_chemical_formula_sum            'C6 H3 Br2 O5 Sb W'
_chemical_formula_weight         620.50
_chemical_name_systematic
; 
 dibromo(methyl)stibine-pentacarbonyltungsten(0) 
;
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-05-23
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record
; 2011-05-28 Relabelled some C & O to match other M(CO)5L
  2011-09-29 Added Sb1...O2' contact. mw
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.5876(10)
_cell_length_b                   12.473(3)
_cell_length_c                   31.209(6)
_cell_measurement_reflns_used    35891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2564.4(9)
_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_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18132
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.300
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5325
_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    3.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0277
_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)+(0.0097P)²+20.3426P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                2604
_reflns_number_total             2951
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om2010996_si_002.cif
_cod_data_source_block           11slb129x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        2564.4(8)
_cod_database_code               4068119
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
W1 W 0.98808(3) 0.384709(17) 0.418410(7) 0.01723(7) Uani 1 1 d .
Sb1 Sb 1.10778(6) 0.44620(3) 0.339510(12) 0.02062(9) Uani 1 1 d .
Br1 Br 0.91849(11) 0.60169(5) 0.30830(2) 0.03300(15) Uani 1 1 d .
Br2 Br 1.00803(11) 0.30592(5) 0.28626(2) 0.03336(16) Uani 1 1 d .
O1 O 0.5615(7) 0.3116(4) 0.38145(15) 0.0334(10) Uani 1 1 d .
O2 O 1.1670(7) 0.1533(3) 0.39745(15) 0.0322(10) Uani 1 1 d .
O3 O 1.4084(7) 0.4538(4) 0.46077(15) 0.0332(10) Uani 1 1 d .
O4 O 0.7944(7) 0.6129(4) 0.43934(16) 0.0368(11) Uani 1 1 d .
O5 O 0.8387(7) 0.3004(4) 0.50824(15) 0.0379(11) Uani 1 1 d .
C1 C 1.3929(9) 0.4837(6) 0.3121(2) 0.0313(14) Uani 1 1 d .
H1A H 1.4667 0.4172 0.3059 0.047 Uiso 1 1 calc R
H1B H 1.4717 0.5273 0.3323 0.047 Uiso 1 1 calc R
H1C H 1.3725 0.5239 0.2855 0.047 Uiso 1 1 calc R
C2 C 0.7161(9) 0.3384(5) 0.3940(2) 0.0258(13) Uani 1 1 d .
C3 C 1.1061(9) 0.2365(5) 0.40491(18) 0.0214(12) Uani 1 1 d .
C4 C 1.2614(9) 0.4307(5) 0.44558(19) 0.0235(12) Uani 1 1 d .
C5 C 0.8663(9) 0.5319(5) 0.4314(2) 0.0249(13) Uani 1 1 d .
C6 C 0.8948(9) 0.3320(5) 0.4757(2) 0.0272(13) 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
W1 0.01769(12) 0.01624(12) 0.01777(13) 0.00097(8) 0.00062(8) -0.00027(8)
Sb1 0.02179(19) 0.02111(18) 0.01896(19) 0.00136(15) 0.00028(15) -0.00079(15)
Br1 0.0391(4) 0.0278(3) 0.0320(4) 0.0051(3) -0.0038(3) 0.0068(3)
Br2 0.0455(4) 0.0292(3) 0.0253(3) -0.0034(3) -0.0022(3) -0.0079(3)
O1 0.024(2) 0.036(2) 0.040(3) -0.006(2) -0.007(2) -0.0019(19)
O2 0.042(3) 0.020(2) 0.035(3) 0.0015(19) 0.003(2) 0.0066(19)
O3 0.026(2) 0.039(3) 0.035(3) -0.005(2) -0.008(2) -0.005(2)
O4 0.039(3) 0.026(2) 0.045(3) -0.007(2) -0.001(2) 0.005(2)
O5 0.044(3) 0.042(3) 0.028(3) 0.006(2) 0.009(2) -0.010(2)
C1 0.022(3) 0.041(4) 0.031(4) -0.001(3) 0.005(3) -0.003(3)
C2 0.027(3) 0.023(3) 0.027(3) -0.005(2) 0.003(3) 0.001(2)
C3 0.022(3) 0.023(3) 0.020(3) 0.005(2) -0.002(2) 0.000(2)
C4 0.022(3) 0.024(3) 0.025(3) -0.002(2) 0.005(2) -0.001(2)
C5 0.025(3) 0.023(3) 0.026(3) 0.001(2) 0.003(3) 0.002(2)
C6 0.025(3) 0.028(3) 0.029(3) -0.003(3) 0.003(3) 0.002(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'
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'
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
C6 W1 C2 88.4(3)
C6 W1 C5 89.8(2)
C2 W1 C5 89.1(2)
C6 W1 C3 90.2(2)
C2 W1 C3 90.0(2)
C5 W1 C3 179.1(2)
C6 W1 C4 89.5(2)
C2 W1 C4 177.9(2)
C5 W1 C4 90.7(2)
C3 W1 C4 90.2(2)
C6 W1 Sb1 177.13(18)
C2 W1 Sb1 89.76(18)
C5 W1 Sb1 92.30(17)
C3 W1 Sb1 87.58(16)
C4 W1 Sb1 92.34(16)
C1 Sb1 Br2 96.86(19)
C1 Sb1 Br1 96.54(19)
Br2 Sb1 Br1 98.78(3)
C1 Sb1 W1 133.72(19)
Br2 Sb1 W1 109.32(2)
Br1 Sb1 W1 115.47(2)
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
O1 C2 W1 177.9(6)
O2 C3 W1 178.4(5)
O3 C4 W1 178.6(6)
O4 C5 W1 178.2(6)
O5 C6 W1 178.6(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 C6 2.002(6)
W1 C2 2.032(6)
W1 C5 2.044(6)
W1 C3 2.049(6)
W1 C4 2.071(6)
W1 Sb1 2.6969(6)
Sb1 C1 2.116(6)
Sb1 Br2 2.5012(8)
Sb1 Br1 2.5031(8)
O1 C2 1.141(7)
O2 C3 1.137(7)
O3 C4 1.116(7)
O4 C5 1.143(7)
O5 C6 1.150(7)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 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 3.484(4) 8_865
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
C2 W1 Sb1 Br1 66.27(17)
C2 W1 Sb1 Br2 -43.98(17)
C2 W1 Sb1 C1 -164.7(3)
C4 W1 Sb1 C1 15.5(3)
