Capped-Tetrahedrally Coordinated Fe(II) and Co(II) Complexes Using a "Click"-Derived Tripodal Ligand: Geometric and Electronic Structures
David Schweinfurth; Serhiy Demeshko; Marat M. Khusniyarov; Sebastian Dechert; Venkatanarayana Gurram; Michael R. Buchmeiser; Franc Meyer; Biprajit Sarkar; Inorganic Chemistry 51 (2012) 7592–7597; doi:10.1021/ic300392e

data_4329697
_publ_section_title
;
 Capped-Tetrahedrally Coordinated Fe(II) and Co(II) Complexes Using a
 "Click"-Derived Tripodal Ligand: Geometric and Electronic Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7592
_journal_page_last               7597
_journal_paper_doi               10.1021/ic300392e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C60 H60 B2 Cl2 Co2 F8 N20'
_chemical_formula_weight         1423.66
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4903(2)
_cell_length_b                   24.7645(5)
_cell_length_c                   12.1277(2)
_cell_measurement_reflns_used    6796
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1.5
_cell_volume                     3751.29(11)
_computing_cell_refinement       'DENZO (W. Minor & Z. Otwinowski)'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'DENZO & SCALEPACK (W. Minor & Z. Otwinowski)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'four-circle, ccd detector'
_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    0.0604
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8897
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SCALEPACK (W. Minor & Z. Otwinowski)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.384(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8897
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0626P)^2^+4.6657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                6796
_reflns_number_total             8897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300392e_si_001.cif
_cod_data_source_block           c:\x-step\dsaug10
_cod_database_code               4329697