Synthesis, X-ray structures and reactivity of calix[5]arene bismuth(iii) and antimony(iii) complexes
Mendoza-Espinosa, Daniel; Hanna, Tracy A.; Dalton Transactions  (2009) 5211–5225; doi:10.1039/b903943k

data_7001567
_publ_section_title
;
 Synthesis, X-ray structures and reactivity of calix[5]arene
 bismuth(iii) and antimony(iii) complexes
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5211
_journal_page_last               5225
_journal_paper_doi               10.1039/b903943k
_journal_year                    2009
_chemical_formula_moiety         'C114 H144 Bi4 O14 S2, 3.5(C2H6SO)'
_chemical_formula_sum            'C121 H165 Bi4 O17.5 S5.5'
_chemical_formula_weight         2911.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 109.8140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6628(13)
_cell_length_b                   33.463(2)
_cell_length_c                   22.8640(16)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     13433.5(16)
_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      223(2)
_diffrn_detector_area_resol_mean 'not recorded'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1009
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91378
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_diffrn_standards_decay_%        'not recorded'
_diffrn_standards_interval_count 'not recorded'
_diffrn_standards_interval_time  'not recorded'
_diffrn_standards_number         'not recorded'
_exptl_absorpt_coefficient_mu    5.304
_exptl_absorpt_correction_T_max  0.5456
_exptl_absorpt_correction_T_min  0.2583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         6.330
_refine_diff_density_min         -7.823
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1210
_refine_ls_number_reflns         24057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.1999
_reflns_number_gt                17260
_reflns_number_total             24057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903943k.txt
_cod_data_source_block           tcu82m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        13433.4(16)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7001567