Cobalt Half-Sandwich, Sandwich, and Mixed Sandwich Complexes with Soft Tripodal Ligands
Christopher A. Dodds; Mario-Alexander Lehmann; Jonathan F. Ojo; John Reglinski; Mark D. Spicer; Inorganic Chemistry 43 (2004) 4927–4934; doi:10.1021/ic0496525

data_4311443
_publ_section_title
;
 Cobalt Half-Sandwich, Sandwich, and Mixed Sandwich Complexes with Soft
 Tripodal Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4927
_journal_page_last               4934
_journal_paper_doi               10.1021/ic0496525
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 B3 Co1 F4 N12 S6'
_chemical_formula_sum            'C25 H35 B3 Co F4 N12 O0.75 S6'
_chemical_formula_weight         875.37
_chemical_name_common            '[Co(Tm)2]BF4. 0.5H2O . 0.25THF'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-10-24T11:40:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0403(7)
_cell_length_b                   12.8344(3)
_cell_length_c                   19.2489(5)
_cell_measurement_reflns_used    9358
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     8239.6(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0048534
_diffrn_orient_matrix_UB_12      0.0724399
_diffrn_orient_matrix_UB_13      0.0154671
_diffrn_orient_matrix_UB_21      0.0290394
_diffrn_orient_matrix_UB_22      0.016667
_diffrn_orient_matrix_UB_23      0.0036614
_diffrn_orient_matrix_UB_31      -0.0056695
_diffrn_orient_matrix_UB_32      0.0233562
_diffrn_orient_matrix_UB_33      -0.0505845
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17044
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.393
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+36.0408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                6799
_reflns_number_total             9437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0496525si20040507_093809_2.cif
_cod_data_source_block           cotm2bf4
_cod_original_formula_sum        'C25 H35 B3 Co1 F4 N12 O0.75 S6'
_cod_database_code               4311443