Synthesis of bismuth and antimony complexes of the “larger” calix[n]arenes (n = 6‒8); from mononuclear to tetranuclear complexes
Mendoza-Espinosa, Daniel; Rheingold, Arnold L.; Hanna, Tracy A.; Dalton Transactions  (2009) 5226–5238; doi:10.1039/b903947c

data_7001561
_publ_section_title
;
 Synthesis of bismuth and antimony complexes of the
 &#x201C;larger&#x201D; calix[n]arenes (n = 6--8); from mononuclear to
 tetranuclear complexes
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5226
_journal_page_last               5238
_journal_paper_doi               10.1039/b903947c
_journal_year                    2009
_chemical_formula_moiety         'C228 H184 Bi8 N2 O21, 4(C6H6)'
_chemical_formula_sum            'C252 H208 Bi8 N2 O21'
_chemical_formula_weight         5272.19
_chemical_name_systematic
;
?
;
_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                92.148(4)
_cell_angle_beta                 90.463(4)
_cell_angle_gamma                112.019(3)
_cell_formula_units_Z            2
_cell_length_a                   19.468(4)
_cell_length_b                   22.096(4)
_cell_length_c                   27.093(6)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     10794(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1229
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51430
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         1.86
_diffrn_standards_interval_count 'not recorded'
_diffrn_standards_interval_time  'not recorded'
_diffrn_standards_number         'not recorded'
_exptl_absorpt_coefficient_mu    6.560
_exptl_absorpt_correction_T_max  0.4200
_exptl_absorpt_correction_T_min  0.3687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5026
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.941
_refine_diff_density_min         -2.372
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1775
_refine_ls_number_reflns         30715
_refine_ls_number_restraints     605
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                18277
_reflns_number_total             30715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903947c.txt
_cod_data_source_block           tcu219m
_cod_depositor_comments
;
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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001561