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_4316924
_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 H33 As0.915 N S6 Sb1.085'
_chemical_formula_weight         896.66
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.4342(7)
_cell_length_b                   11.4342(7)
_cell_length_c                   16.131(2)
_cell_measurement_reflns_used    3150
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.73
_cell_measurement_theta_min      2.41
_cell_volume                     1826.4(3)
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18014
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    2.012
_exptl_absorpt_correction_T_max  0.8720
_exptl_absorpt_correction_T_min  0.4854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             899
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1387
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0380P)^2^+0.2129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                1226
_reflns_number_total             1387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1012186_si_002.cif
_cod_data_source_block           g41
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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 
;
_cod_original_cell_volume        1826.5(3)
_cod_database_code               4316924