#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/65/2216511.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2216511
loop_
_publ_author_name
'Yanlong Sun'
'Yantuan Li'
'Xin Cui'
'Xiuting Lang'
_publ_section_title
Bromidobis(morpholine-4-dithiocarboxylato-κ²S,S')antimony(III)
_journal_coeditor_code           HB2665
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3132
_journal_page_last               m3132
_journal_paper_doi               10.1107/S1600536807060382
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Sb Br (C5 H8 N O S2)2]'
_chemical_formula_moiety         'C10 H16 Br N2 O2 S4 Sb'
_chemical_formula_sum            'C10 H16 Br N2 O2 S4 Sb'
_chemical_formula_weight         526.15
_chemical_name_systematic
;
Bromidobis(morpholine-4-dithiocarboxylato-κ²S,S')antimony(III)
;
_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                71.060(4)
_cell_angle_beta                 81.796(4)
_cell_angle_gamma                76.924(3)
_cell_formula_units_Z            2
_cell_length_a                   6.428(2)
_cell_length_b                   11.175(4)
_cell_length_c                   13.241(4)
_cell_measurement_reflns_used    2859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.981
_cell_measurement_theta_min      2.909
_cell_volume                     873.8(5)
_computing_cell_refinement       'SAINT (Bruker 1998)'
_computing_data_collection       'SMART (Bruker 1998)'
_computing_data_reduction        'SAINT (Bruker 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker 1998)'
_computing_publication_material  'SHELXL97 (Bruker 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4592
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.343
_exptl_absorpt_correction_T_max  0.257
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.43
_refine_diff_density_max         2.018
_refine_diff_density_min         -1.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0961P)²+5.9643P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1602
_reflns_number_gt                2616
_reflns_number_total             3044
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2665.cif
_cod_data_source_block           I
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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_database_code               2216511
_cod_database_fobs_code          2216511
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Sb Sb1 -0.00045(9) 0.46615(5) 0.32671(4) 0.0291(2) Uani d . 1
Br Br1 0.16432(17) 0.69319(9) 0.27216(8) 0.0455(3) Uani d . 1
N N1 0.2808(12) 0.1526(7) 0.5928(6) 0.0327(16) Uani d . 1
N N2 0.2041(11) 0.3082(7) 0.0529(6) 0.0326(16) Uani d . 1
O O1 0.5164(13) -0.0596(7) 0.7403(6) 0.0519(18) Uani d . 1
O O2 0.3961(12) 0.1478(7) -0.0739(5) 0.0477(17) Uani d . 1
S S1 0.2747(4) 0.3940(2) 0.46525(18) 0.0347(5) Uani d . 1
S S2 0.0126(4) 0.2235(2) 0.43813(19) 0.0402(6) Uani d . 1
S S3 0.2845(3) 0.4096(2) 0.19460(18) 0.0336(5) Uani d . 1
S S4 -0.1470(3) 0.3730(2) 0.17329(19) 0.0375(5) Uani d . 1
C C1 0.1961(13) 0.2443(8) 0.5102(7) 0.0299(18) Uani d . 1
C C2 0.4261(16) 0.1714(9) 0.6596(8) 0.041(2) Uani d . 1
H H2A 0.3463 0.1874 0.7234 0.049 Uiso calc R 1
H H2B 0.4890 0.2461 0.6204 0.049 Uiso calc R 1
C C3 0.6012(17) 0.0538(9) 0.6913(9) 0.047(2) Uani d . 1
H H3A 0.6928 0.0451 0.6282 0.056 Uiso calc R 1
H H3B 0.6882 0.0647 0.7406 0.056 Uiso calc R 1
C C4 0.3955(18) -0.0798(9) 0.6673(9) 0.048(3) Uani d . 1
H H4A 0.3447 -0.1602 0.6996 0.057 Uiso calc R 1
H H4B 0.4857 -0.0857 0.6031 0.057 Uiso calc R 1
C C5 0.2063(16) 0.0308(9) 0.6381(8) 0.042(2) Uani d . 1
H H5A 0.1272 0.0182 0.5864 0.050 Uiso calc R 1
H H5B 0.1108 0.0329 0.7015 0.050 Uiso calc R 1
C C6 0.1182(13) 0.3570(7) 0.1320(6) 0.0270(17) Uani d . 1
C C7 0.4269(14) 0.3060(9) 0.0091(8) 0.038(2) Uani d . 1
H H7A 0.5094 0.3198 0.0588 0.046 Uiso calc R 1
H H7B 0.4328 0.3750 -0.0579 0.046 Uiso calc R 1
C C8 0.5227(16) 0.1772(9) -0.0101(8) 0.041(2) Uani d . 1
H H8A 0.6655 0.1798 -0.0452 0.049 Uiso calc R 1
H H8B 0.5349 0.1099 0.0582 0.049 Uiso calc R 1
C C9 0.1872(17) 0.1407(10) -0.0235(8) 0.046(2) Uani d . 1
H H9A 0.1969 0.0745 0.0455 0.055 Uiso calc R 1
H H9B 0.1049 0.1163 -0.0670 0.055 Uiso calc R 1
C C10 0.0739(17) 0.2665(11) -0.0077(9) 0.049(3) Uani d . 1
H H10A 0.0500 0.3311 -0.0767 0.059 Uiso calc R 1
H H10B -0.0643 0.2572 0.0311 0.059 Uiso calc R 1
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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_publ_flag
S3 Sb1 S1 89.32(8) y
S3 Sb1 S2 92.18(8) y
S1 Sb1 S2 69.49(7) y
S3 Sb1 Br1 83.76(6) y
S1 Sb1 Br1 80.99(6) y
S2 Sb1 Br1 150.27(6) y
S3 Sb1 S4 66.17(7) y
S1 Sb1 S4 139.75(7) y
S2 Sb1 S4 79.63(7) y
Br1 Sb1 S4 124.28(6) y
C1 N1 C5 122.2(8) ?
C1 N1 C2 123.5(7) ?
C5 N1 C2 113.3(7) ?
C6 N2 C7 123.8(7) ?
C6 N2 C10 122.0(7) ?
C7 N2 C10 113.7(7) ?
C3 O1 C4 110.0(7) ?
C8 O2 C9 110.7(7) ?
C1 S1 Sb1 87.9(3) ?
C1 S2 Sb1 86.0(3) ?
C6 S3 Sb1 94.4(3) ?
C6 S4 Sb1 80.8(3) ?
N1 C1 S2 122.9(6) ?
N1 C1 S1 120.7(6) ?
S2 C1 S1 116.3(5) ?
N1 C2 C3 110.4(7) ?
N1 C2 H2A 109.6 ?
C3 C2 H2A 109.6 ?
N1 C2 H2B 109.6 ?
C3 C2 H2B 109.6 ?
H2A C2 H2B 108.1 ?
O1 C3 C2 111.6(8) ?
O1 C3 H3A 109.3 ?
C2 C3 H3A 109.3 ?
O1 C3 H3B 109.3 ?
C2 C3 H3B 109.3 ?
H3A C3 H3B 108.0 ?
O1 C4 C5 109.9(9) ?
O1 C4 H4A 109.7 ?
C5 C4 H4A 109.7 ?
O1 C4 H4B 109.7 ?
C5 C4 H4B 109.7 ?
H4A C4 H4B 108.2 ?
N1 C5 C4 110.0(8) ?
N1 C5 H5A 109.7 ?
C4 C5 H5A 109.7 ?
N1 C5 H5B 109.7 ?
C4 C5 H5B 109.7 ?
H5A C5 H5B 108.2 ?
N2 C6 S4 123.2(6) ?
N2 C6 S3 118.3(6) ?
S4 C6 S3 118.5(5) ?
N2 C7 C8 110.1(7) ?
N2 C7 H7A 109.6 ?
C8 C7 H7A 109.6 ?
N2 C7 H7B 109.6 ?
C8 C7 H7B 109.6 ?
H7A C7 H7B 108.1 ?
O2 C8 C7 111.4(8) ?
O2 C8 H8A 109.3 ?
C7 C8 H8A 109.3 ?
O2 C8 H8B 109.3 ?
C7 C8 H8B 109.3 ?
H8A C8 H8B 108.0 ?
O2 C9 C10 111.6(9) ?
O2 C9 H9A 109.3 ?
C10 C9 H9A 109.3 ?
O2 C9 H9B 109.3 ?
C10 C9 H9B 109.3 ?
H9A C9 H9B 108.0 ?
N2 C10 C9 109.7(8) ?
N2 C10 H10A 109.7 ?
C9 C10 H10A 109.7 ?
N2 C10 H10B 109.7 ?
C9 C10 H10B 109.7 ?
H10A C10 H10B 108.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sb1 S3 2.469(2) y
Sb1 S1 2.542(2) y
Sb1 S2 2.621(2) y
Sb1 S4 2.909(2) y
Sb1 Br1 2.8087(14) y
N1 C1 1.317(11) ?
N1 C5 1.458(11) ?
N1 C2 1.464(12) ?
N2 C6 1.330(11) ?
N2 C7 1.464(11) ?
N2 C10 1.474(12) ?
O1 C3 1.414(12) ?
O1 C4 1.423(12) ?
O2 C8 1.408(12) ?
O2 C9 1.419(12) ?
S1 C1 1.748(9) ?
S2 C1 1.716(9) ?
S3 C6 1.740(8) ?
S4 C6 1.702(8) ?
C2 C3 1.510(13) ?
C2 H2A 0.9700 ?
C2 H2B 0.9700 ?
C3 H3A 0.9700 ?
C3 H3B 0.9700 ?
C4 C5 1.517(14) ?
C4 H4A 0.9700 ?
C4 H4B 0.9700 ?
C5 H5A 0.9700 ?
C5 H5B 0.9700 ?
C7 C8 1.518(13) ?
C7 H7A 0.9700 ?
C7 H7B 0.9700 ?
C8 H8A 0.9700 ?
C8 H8B 0.9700 ?
C9 C10 1.495(14) ?
C9 H9A 0.9700 ?
C9 H9B 0.9700 ?
C10 H10A 0.9700 ?
C10 H10B 0.9700 ?
