Highly labile cationic tris-acetonitrile complexes, [TpRM(NCMe)3]OTf (M = Ni, Co; TpR: hydrotrispyrazolylborato, R = Ph, Me and iPr2): versatile precursors for TpR-containing nickel and cobalt complexes
Uehara, Kazuhiro; Hikichi, Shiro; Akita, Munetaka; Journal of the Chemical Society, Dalton Transactions  (2002) 3529–; doi:10.1039/b203377c

data_7011717
_publ_section_title
;
 Highly labile cationic tris-acetonitrile complexes, [TpRM(NCMe)3]OTf
 (M = Ni, Co; TpR: hydrotrispyrazolylborato, R = Ph, Me and iPr2):
 versatile precursors for TpR-containing nickel and cobalt complexes
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3529
_journal_paper_doi               10.1039/b203377c
_journal_year                    2002
_chemical_formula_moiety         'C44 H70 B F3 N14 O3 Ni S '
_chemical_formula_sum            'C44 H70 B F3 N14 Ni O3 S'
_chemical_formula_weight         1001.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Jun 26 02:11:20 2002'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                102.376(5)
_cell_angle_beta                 113.607(7)
_cell_angle_gamma                85.327(6)
_cell_formula_units_Z            2
_cell_length_a                   11.928(2)
_cell_length_b                   22.496(2)
_cell_length_c                   11.717(1)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    213.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.9
_cell_volume                     2814.0(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20462
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.34
_refine_diff_density_min         -1.38
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.499
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     648
_refine_ls_number_reflns         8223
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          -0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2438
_reflns_number_gt                8223
_reflns_number_total             11372
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            b203377c.txt
_cod_data_source_block           compound_1'Ni
_cod_original_cell_volume        2813.8(6)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C44 H70 B F3 N14 O3 Ni S '
_cod_database_code               7011717