Facile Synthesis of Bismuth(III) and Antimony(III) Complexes Supported by Silylated Calix[5]arenes.
Daniel Mendoza-Espinosa; Tracy A. Hanna; Inorganic Chemistry 48 (2009) 10312–10325; doi:10.1021/ic9014477

data_4303498
_publ_section_title
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Facile Synthesis of Bismuth(III) and Antimony(III) Complexes Supported by
Silylated Calix[5]arenes.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10312
_journal_page_last               10325
_journal_paper_doi               10.1021/ic9014477
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C66 H85 Bi O7 S2 Si,C2H6OS'
_chemical_formula_sum            'C68 H91 Bi O8 S3 Si'
_chemical_formula_weight         1369.66
_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                112.877(4)
_cell_angle_beta                 92.901(4)
_cell_angle_gamma                102.414(4)
_cell_formula_units_Z            2
_cell_length_a                   11.377(3)
_cell_length_b                   17.416(4)
_cell_length_c                   20.856(4)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3676.8(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_detector_area_resol_mean 'not recorded'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1839
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14957
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.85
_diffrn_standards_interval_count 'not recorded'
_diffrn_standards_interval_time  'not recorded'
_diffrn_standards_number         'not recorded'
_exptl_absorpt_coefficient_mu    2.546
_exptl_absorpt_correction_T_max  0.7170
_exptl_absorpt_correction_T_min  0.6169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.338
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         10473
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                6317
_reflns_number_total             10473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9014477_si_001_04.cif
_cod_data_source_block           tcu202m
_cod_depositor_comments
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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 
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_cod_database_code               4303498