Equilibrium Studies in Solution Involving Nickel(II) Complexes of Flexidentate Schiff Base Ligands: Isolation and Structural Characterization of the Planar Red and Octahedral Green Species Involved in the Equilibrium
Suman Mukhopadhyay; Debdas Mandal; Dipesh Ghosh; Israel Goldberg; Muktimoy Chaudhury; Inorganic Chemistry 42 (2003) 8439–8445; doi:10.1021/ic0346174

data_4312678
_publ_section_title
;
 Equilibrium Studies in Solution Involving Nickel(II) Complexes of
 Flexidentate Schiff Base Ligands: Isolation and Structural
 Characterization of the Planar Red and Octahedral Green Species Involved
 in the Equilibrium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8439
_journal_page_last               8445
_journal_paper_doi               10.1021/ic0346174
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C37 H37 B Br N3 Ni O'
_chemical_formula_weight         689.13
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.72900(10)
_cell_length_b                   9.72900(10)
_cell_length_c                   56.9660(13)
_cell_measurement_reflns_used    4041
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.42
_cell_volume                     4669.63(13)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF-96
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.5 deg. Omega scans'
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            9496
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  0.8295
_exptl_absorpt_correction_T_min  0.6974
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallelpiped rods'
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.478(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+9.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                4041
_reflns_number_total             5407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0346174si20030604_081154_4.cif
_cod_data_source_block           Compound-3
_cod_database_code               4312678