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_4324995
_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            'C85.5 H115.5 K2 N12.5 Ni2 O19.5'
_chemical_formula_weight         1826.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 112.8460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.2311(4)
_cell_length_b                   35.1796(6)
_cell_length_c                   27.2846(5)
_cell_measurement_reflns_used    9408
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      2.52
_cell_volume                     19664.8(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            180344
_diffrn_reflns_theta_full        67.73
_diffrn_reflns_theta_max         67.73
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  0.6147
_exptl_absorpt_correction_T_min  0.4985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             7728
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.306(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2956
_refine_ls_number_reflns         32284
_refine_ls_number_restraints     7916
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1318P)^2^+7.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                28726
_reflns_number_total             32284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200143b_si_005.cif
_cod_data_source_block           d09035_sq
_cod_original_formula_sum        'C85.50 H115.50 K2 N12.50 Ni2 O19.50'
_cod_database_code               4324995