Structural and spectroscopic characterisation of bis-ligand complexes of iron(ii), nickel(ii) and nickel(iii) with the hydrotris(methimazolyl)borate anion: soft S6 donor sets generating a weak ligand field
Garner, Mark; Lewinski, Krzysztof; Pattek-Janczyk, Agnieszka; Reglinski, John; Sieklucka, Barbara; Spicer, Mark D.; Szaleniec, Maciej; Dalton Transactions  (2003) 1181–; doi:10.1039/b209877f

data_7012309
_publ_section_title
;
 Structural and spectroscopic characterisation of bis-ligand complexes
 of iron(ii), nickel(ii) and nickel(iii) with the
 hydrotris(methimazolyl)borate anion: soft S6 donor sets generating a
 weak ligand field
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1181
_journal_paper_doi               10.1039/b209877f
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 B2 Br1 N12 Ni1 S6, 4(C H2 CL2)'
_chemical_formula_sum            'C28 H40 B2 Br Cl8 N12 Ni S6'
_chemical_formula_weight         1180.92
_chemical_name_common            '[Ni(Tm)2]Br.4(CH2Cl2)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      198
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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             2002-11-21T10:11:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8111(4)
_cell_length_b                   16.8111(4)
_cell_length_c                   16.8111(4)
_cell_measurement_reflns_used    1778
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.455
_cell_measurement_wavelength     0.71073
_cell_volume                     4751.0(2)
_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
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0141452
_diffrn_orient_matrix_UB_12      0.0302774
_diffrn_orient_matrix_UB_13      0.0492097
_diffrn_orient_matrix_UB_21      -0.0153822
_diffrn_orient_matrix_UB_22      -0.0468612
_diffrn_orient_matrix_UB_23      0.0332539
_diffrn_orient_matrix_UB_31      0.055693
_diffrn_orient_matrix_UB_32      -0.0206329
_diffrn_orient_matrix_UB_33      -0.003314
_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
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       2
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1771
_diffrn_reflns_theta_full        26.26
_diffrn_reflns_theta_max         26.26
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+31.5216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                1660
_reflns_number_total             1771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b209877f.txt
_cod_data_source_block           nitm2br
_cod_original_sg_symbol_H-M      P213
_cod_original_formula_sum        'C28 H40 B2 Br1 Cl8 N12 Ni1 S6'
_cod_database_code               7012309