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_4324993
_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            'C121 H180 Fe2 K3 N9 O36'
_chemical_formula_weight         2565.74
_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                92.8330(10)
_cell_angle_beta                 90.3590(10)
_cell_angle_gamma                115.2440(10)
_cell_formula_units_Z            2
_cell_length_a                   15.0668(2)
_cell_length_b                   17.0823(3)
_cell_length_c                   29.0767(5)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.71
_cell_measurement_theta_min      2.86
_cell_volume                     6757.6(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            135866
_diffrn_reflns_theta_full        67.73
_diffrn_reflns_theta_max         67.73
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_T_max  0.5406
_exptl_absorpt_correction_T_min  0.3478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2298
_refine_ls_number_reflns         23812
_refine_ls_number_restraints     11137
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0781
_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^)+(0.1210P)^2^+6.6402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2137
_refine_ls_wR_factor_ref         0.2289
_reflns_number_gt                17080
_reflns_number_total             23812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200143b_si_003.cif
_cod_data_source_block           d10029_sq
_cod_original_cell_volume        6757.57(19)
_cod_database_code               4324993