#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:05:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179276 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/96/4319687.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_4319687
loop_
_publ_author_name
'Narcis Avarvari'
'Eric Faulques'
'Marc Fourmigué'
_publ_section_title
;
 Two Successive Single Crystal Phase Transitions Involving the
 Coordination Sphere of Antimony in PhSb(dmit), the First
 Organo-Antimony(III) Dithiolene Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2570
_journal_page_last               2577
_journal_paper_doi               10.1021/ic001439v
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H13 O S5 Sb'
_chemical_formula_weight         467.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.580(3)
_cell_length_b                   8.9756(18)
_cell_length_c                   15.905(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     1697.4(7)
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.5'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3274
_diffrn_reflns_theta_full        25.89
_diffrn_reflns_theta_max         25.89
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  0.8471
_exptl_absorpt_correction_T_min  0.5603
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   faceit
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0463P)²+0.2831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                2753
_reflns_number_total             3274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001439v_1.cif
_cod_data_source_block           PhSb(dmit)_RT
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1697.5(6)
_cod_database_code               4319687
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
Sb1 Sb 0.167900(17) 0.05543(2) 0.075786(14) 0.03708(9) Uani 1 1 d . . .
S1 S 0.03076(7) 0.18834(9) 0.13025(7) 0.0432(2) Uani 1 1 d . . .
S2 S 0.23144(7) 0.31041(10) 0.04256(6) 0.0437(2) Uani 1 1 d . . .
S3 S -0.00411(7) 0.50979(9) 0.15640(6) 0.03851(19) Uani 1 1 d . . .
S4 S 0.16754(7) 0.61298(10) 0.08811(6) 0.0418(2) Uani 1 1 d . . .
S5 S 0.03148(9) 0.83392(10) 0.15136(7) 0.0504(2) Uani 1 1 d . . .
C1 C 0.0704(2) 0.3724(3) 0.12190(19) 0.0313(6) Uani 1 1 d . . .
C2 C 0.1503(3) 0.4195(3) 0.08821(19) 0.0342(7) Uani 1 1 d . . .
C3 C 0.0638(3) 0.6605(3) 0.1315(2) 0.0364(7) Uani 1 1 d . . .
C4 C 0.3002(3) 0.0341(4) 0.2028(2) 0.0462(8) Uani 1 1 d . . .
C5 C 0.2950(4) 0.0935(6) 0.2806(3) 0.0708(13) Uani 1 1 d . . .
H5 H 0.2314 0.1459 0.2811 0.085 Uiso 1 1 calc R . .
C6 C 0.3854(5) 0.0757(7) 0.3595(3) 0.096(2) Uani 1 1 d . . .
H6 H 0.3812 0.1166 0.4120 0.115 Uiso 1 1 calc R . .
C7 C 0.4785(5) 0.0001(8) 0.3604(4) 0.0972(19) Uani 1 1 d . . .
H7 H 0.5391 -0.0076 0.4128 0.117 Uiso 1 1 calc R . .
C8 C 0.4834(4) -0.0652(9) 0.2839(4) 0.109(3) Uani 1 1 d . . .
H8 H 0.5464 -0.1200 0.2846 0.131 Uiso 1 1 calc R . .
C9 C 0.3925(4) -0.0491(7) 0.2041(3) 0.0838(18) Uani 1 1 d . . .
H9 H 0.3951 -0.0948 0.1523 0.101 Uiso 1 1 calc R . .
O1 O 0.6663(5) 0.0345(6) 0.0156(3) 0.1137(16) Uani 1 1 d . . .
C10 C 0.6689(10) -0.0540(9) 0.0827(6) 0.161(5) Uani 1 1 d . . .
H10A H 0.7235 -0.1326 0.0877 0.193 Uiso 1 1 calc R . .
H10B H 0.5957 -0.0999 0.0713 0.193 Uiso 1 1 calc R . .
C11 C 0.6968(12) 0.0239(12) 0.1615(5) 0.182(5) Uani 1 1 d . . .
H11A H 0.6364 0.0162 0.1866 0.218 Uiso 1 1 calc R . .
H11B H 0.7642 -0.0184 0.2037 0.218 Uiso 1 1 calc R . .
C12 C 0.7149(8) 0.1688(10) 0.1470(5) 0.137(3) Uani 1 1 d . . .
H12A H 0.7941 0.1931 0.1724 0.165 Uiso 1 1 calc R . .
H12B H 0.6724 0.2332 0.1734 0.165 Uiso 1 1 calc R . .
C13 C 0.6769(9) 0.1863(10) 0.0507(6) 0.149(4) Uani 1 1 d . . .
H13A H 0.7312 0.2425 0.0321 0.178 Uiso 1 1 calc R . .
H13B H 0.6051 0.2375 0.0302 0.178 Uiso 1 1 calc R . .
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'
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
C4 Sb1 S1 97.30(11) . . ?
C4 Sb1 S2 94.34(10) . . ?
S1 Sb1 S2 86.63(3) . . ?
C4 Sb1 O1 89.10(14) . 3_655 ?
S1 Sb1 O1 165.60(11) . 3_655 ?
S2 Sb1 O1 80.01(11) . 3_655 ?
C4 Sb1 S5 86.32(10) . 1_545 ?
S1 Sb1 S5 68.75(3) . 1_545 ?
S2 Sb1 S5 155.21(3) . 1_545 ?
O1 Sb1 S5 124.77(11) 3_655 1_545 ?
C4 Sb1 S5 168.07(10) . 3_565 ?
S1 Sb1 S5 83.54(3) . 3_565 ?
S2 Sb1 S5 73.79(3) . 3_565 ?
O1 Sb1 S5 87.56(10) 3_655 3_565 ?
S5 Sb1 S5 104.97(3) 1_545 3_565 ?
C4 Sb1 Sb1 145.94(10) . 3 ?
S1 Sb1 Sb1 68.49(3) . 3 ?
S2 Sb1 Sb1 114.61(2) . 3 ?
O1 Sb1 Sb1 112.36(9) 3_655 3 ?
S5 Sb1 Sb1 59.83(2) 1_545 3 ?
S5 Sb1 Sb1 45.14(2) 3_565 3 ?
C1 S1 Sb1 100.40(11) . . ?
C2 S2 Sb1 98.83(11) . . ?
C3 S3 C1 97.20(16) . . ?
C3 S4 C2 97.78(15) . . ?
C2 C1 S3 116.7(2) . . ?
C2 C1 S1 126.5(2) . . ?
S3 C1 S1 116.71(18) . . ?
C1 C2 S2 127.2(2) . . ?
C1 C2 S4 114.8(2) . . ?
S2 C2 S4 117.99(19) . . ?
S5 C3 S3 121.5(2) . . ?
S5 C3 S4 125.0(2) . . ?
S3 C3 S4 113.48(18) . . ?
C5 C4 C9 119.2(4) . . ?
C5 C4 Sb1 124.1(3) . . ?
C9 C4 Sb1 116.7(3) . . ?
C4 C5 C6 120.1(5) . . ?
C7 C6 C5 121.0(5) . . ?
C6 C7 C8 119.8(4) . . ?
C7 C8 C9 119.8(5) . . ?
C4 C9 C8 120.0(5) . . ?
C10 O1 C13 106.0(5) . . ?
O1 C10 C11 111.2(8) . . ?
C12 C11 C10 109.9(8) . . ?
C11 C12 C13 105.5(7) . . ?
C12 C13 O1 105.0(6) . . ?
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
Sb1 C4 2.166(3) . ?
Sb1 S1 2.4751(10) . ?
Sb1 S2 2.5361(10) . ?
Sb1 O1 3.015(5) 3_655 ?
Sb1 S5 3.1130(11) 1_545 ?
Sb1 S5 3.7964(17) 3_565 ?
Sb1 Sb1 4.2423(14) 3 ?
S1 C1 1.744(3) . ?
S2 C2 1.736(3) . ?
S3 C3 1.714(3) . ?
S3 C1 1.743(3) . ?
S4 C3 1.717(4) . ?
S4 C2 1.750(3) . ?
S5 C3 1.665(3) . ?
C1 C2 1.351(5) . ?
C4 C5 1.368(6) . ?
C4 C9 1.376(6) . ?
C5 C6 1.400(6) . ?
C6 C7 1.349(9) . ?
C7 C8 1.370(9) . ?
C8 C9 1.412(7) . ?
O1 C10 1.323(8) . ?
O1 C13 1.462(10) . ?
C10 C11 1.376(11) . ?
C11 C12 1.352(11) . ?
C12 C13 1.457(10) . ?
