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_7001556
_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         'C84 H66 Bi2 O12,7(C4 H8 O), 2(H2O)'
_chemical_formula_sum            'C112 H126 Bi2 O21'
_chemical_formula_weight         2226.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.940(3)
_cell_length_b                   24.307(5)
_cell_length_c                   29.061(7)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     9847(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      213(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  0.1790
_diffrn_reflns_av_sigmaI/netI    0.1632
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38534
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.82
_diffrn_standards_interval_count 'not recorded'
_diffrn_standards_interval_time  'not recorded'
_diffrn_standards_number         'not recorded'
_exptl_absorpt_coefficient_mu    3.642
_exptl_absorpt_correction_T_max  0.6296
_exptl_absorpt_correction_T_min  0.5446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7102
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                3229
_reflns_number_total             7102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903947c.txt
_cod_data_source_block           tcu177m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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      Pccn
_cod_database_code               7001556