Two Successive Single Crystal Phase Transitions Involving the Coordination Sphere of Antimony in PhSb(dmit), the First Organo-Antimony(III) Dithiolene Complex
Narcis Avarvari; Eric Faulques; Marc Fourmigué; Inorganic Chemistry 40 (2001) 2570–2577; doi:10.1021/ic001439v

data_4319689
_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                 91.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   16.736(3)
_cell_length_b                   8.9653(18)
_cell_length_c                   33.132(7)
_cell_measurement_reflns_used    7997
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     4968.3(17)
_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      180(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 0.7'
_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    0.0188
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9226
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  0.8402
_exptl_absorpt_correction_T_min  0.5246
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   faceit
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.213
_refine_diff_density_min         -11.553
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9226
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.1029
_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/[\s^2^(Fo^2^)+(0.1166P)^2^+192.2551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2682
_refine_ls_wR_factor_ref         0.2813
_reflns_number_gt                7288
_reflns_number_total             9226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001439v_3.cif
_cod_data_source_block           PhSb(dmit)_180K
_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        4968.2(17)
_cod_database_code               4319689