Octanuclear cobalt and nickel cages featuring formate ligands
Cadiou, Cyril; Coxall, Robert A.; Graham, Alasdair; Harrison, Andrew; Helliwell, Madeleine; Parsons, Simon; Winpenny, Richard E. P.; Chemical Communications  (2002) 1106–; doi:10.1039/b202062a

data_7114232
_publ_section_title
;
 Octanuclear cobalt and nickel cages featuring formate ligands
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              1106
_journal_paper_doi               10.1039/b202062a
_journal_year                    2002
_chemical_formula_moiety         '[Ni7Cl2(OH)2(Hmhp)6(TPA)8(HCO2)2].5CH2Cl2'
_chemical_formula_sum            'C203 H176 Cl12 N6 Ni7 O28'
_chemical_formula_weight         3983.87
_space_group_IT_number           2
_symmetry_cell_setting           'Triclinic, twinned via 2[001]*'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.986(15)
_cell_angle_beta                 81.437(18)
_cell_angle_gamma                78.429(12)
_cell_formula_units_Z            1
_cell_length_a                   14.799(9)
_cell_length_b                   16.541(9)
_cell_length_c                   22.688(12)
_cell_measurement_reflns_used    577
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      2
_cell_volume                     5270(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.427
_diffrn_measured_fraction_theta_max 0.427
_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       Omega
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1853
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10488
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   'Not yet available for this kind of twin'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10488
_refine_ls_number_restraints     640
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1490
_refine_ls_R_factor_gt           0.1079
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1889P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3072
_refine_ls_wR_factor_ref         0.3220
_reflns_number_gt                6041
_reflns_number_total             10488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202062a.txt
_cod_data_source_block           niag23
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114232