A rigid cavity containing tetra-cobalt(III) [2 × 2] grid complex
Plante, Jeffrey P.; Jones, Paul D.; Powell, Douglas R.; Glass, Timothy E.; Chemical Communications (Cambridge, United Kingdom)  (2003) 336–337; doi:10.1039/b207039a

data_7103942
_publ_section_title
;
 A rigid cavity containing tetra-cobalt(III) [2 \\times 2] grid complex
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   3
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              336
_journal_page_last               337
_journal_paper_doi               10.1039/b207039a
_journal_year                    2003
_chemical_formula_moiety
'(C112 H64 Co4 N24 O8) 6+, 6(P F6) 1-, 7.12(C3 H6 O), 4.88(C6 H6)'
_chemical_formula_sum            'C162.67 H136 Co4 F36 N24 O15.11 P6'
_chemical_formula_weight         3774.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 113.855(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.027(4)
_cell_length_b                   13.9229(13)
_cell_length_c                   32.327(3)
_cell_measurement_reflns_used    3648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.23
_cell_volume                     16065(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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker APEX'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scan frames'
_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  0.0974
_diffrn_reflns_av_sigmaI/netI    0.1082
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            44663
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        -0.15
_diffrn_standards_number         93
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7692
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         14083
_refine_ls_number_restraints     948
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1899
_refine_ls_R_factor_gt           0.0955
_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^)+(0.1520P)^2^+49.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2503
_refine_ls_wR_factor_ref         0.3067
_reflns_number_gt                6667
_reflns_number_total             14083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207039a.txt
_cod_data_source_block           02044
_cod_database_code               7103942