Self-Assembled E2L3 Cryptands (E = P, As, Sb, Bi): Transmetalation, Homo- and Heterometallic Assemblies, and Conformational Isomerism
Virginia M. Cangelosi; Timothy G. Carter; Justin L. Crossland; Lev N. Zakharov; Darren W. Johnson; Inorganic Chemistry 49 (2010) 9985–9992; doi:10.1021/ic1012186

data_4316925
_publ_section_title
;
 Self-Assembled E2L3 Cryptands (E = P, As, Sb, Bi): Transmetalation, Homo-
 and Heterometallic Assemblies, and Conformational Isomerism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9985
_journal_page_last               9992
_journal_paper_doi               10.1021/ic1012186
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C38 H32 As Bi Cl6 S6'
_chemical_formula_weight         1177.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXLTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4744(8)
_cell_length_b                   16.4744(8)
_cell_length_c                   16.4744(8)
_cell_measurement_reflns_used    2587
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.23
_cell_measurement_theta_min      2.47
_cell_volume                     4471.2(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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector Bruker Apex'
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9348
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.344
_exptl_absorpt_correction_T_max  0.6448
_exptl_absorpt_correction_T_min  0.4636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.040(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3177
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2747
_reflns_number_total             3177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1012186_si_003.cif
_cod_data_source_block           h42c
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4316925