Supramolecular associations in binary antimony(iii) dithiocarbamates: influence of ligand steric bulk, influence on coordination geometry, and competition with hydrogen-bonding
Liu, Yu; Tiekink, Edward R. T.; CrystEngComm 7 (2005) 20–; doi:10.1039/b416493h

data_7203695
_publ_section_title
;
 Supramolecular associations in binary antimony(iii) dithiocarbamates:
 influence of ligand steric bulk, influence on coordination geometry,
 and competition with hydrogen-bonding
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              20
_journal_paper_doi               10.1039/b416493h
_journal_volume                  7
_journal_year                    2005
_chemical_formula_sum            'C21 H36 N3 S6 Sb'
_chemical_formula_weight         644.64
_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
_cell_angle_beta                 99.305(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9080(6)
_cell_length_b                   13.5802(7)
_cell_length_c                   18.8708(10)
_cell_measurement_reflns_used    1985
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      2.4
_cell_volume                     2758.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'Bruker SHEXLTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.082
_diffrn_reflns_av_sigmaI/netI    0.107
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23109
_diffrn_reflns_theta_full        30.1
_diffrn_reflns_theta_max         30.1
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.51
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         8047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.135
_refine_ls_R_factor_gt           0.071
_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^)+(0.046P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.115
_refine_ls_wR_factor_ref         0.135
_reflns_number_gt                4663
_reflns_number_total             8047
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b416493h.txt
_cod_data_source_block           Sb{S2CN(CH2)6}3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7203695