Family of Cofacial Bimetallic Complexes of a Hexaanionic Carboxamide Cryptand
Glen E. Alliger; Peter Müller; Loi H. Do; Christopher C. Cummins; Daniel G. Nocera; Inorganic Chemistry 50 (2011) 4107–4115; doi:10.1021/ic200143b

data_4324992
_publ_section_title
;
 Family of Cofacial Bimetallic Complexes of a Hexaanionic Carboxamide
 Cryptand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4107
_journal_page_last               4115
_journal_paper_doi               10.1021/ic200143b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C81.8 H110.69 N8 O17.45'
_chemical_formula_weight         1485.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.9650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0915(2)
_cell_length_b                   15.5264(2)
_cell_length_c                   32.1740(4)
_cell_measurement_temperature    100(2)
_cell_volume                     8027.69(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            141167
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.7662
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         14686
_refine_ls_number_restraints     2058
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+8.3546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                12309
_reflns_number_total             14686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200143b_si_002.cif
_cod_data_source_block           09043
_cod_original_cell_volume        8027.69(17)
_cod_original_formula_sum        'C81.80 H110.69 N8 O17.45'
_cod_database_code               4324992