Transition Metal Complexes of 3-Cyano- and 3-Nitroformazans
Joe B. Gilroy; Brian O. Patrick; Robert McDonald; Robin G. Hicks; Inorganic Chemistry 47 (2008) 1287–1294; doi:10.1021/ic7019846

data_4304486
_publ_section_title
;
Transition Metal Complexes of 3-Cyano- and 3-Nitroformazans
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1287
_journal_page_last               1294
_journal_paper_doi               10.1021/ic7019846
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C37.5 H40.5 Cl2.5 N10 Ni2 O2'
_chemical_formula_weight         869.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 132.934(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.3752(8)
_cell_length_b                   16.4725(8)
_cell_length_c                   10.6976(5)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.49
_cell_volume                     1983.63(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area 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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14704
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+3.3119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1007
_reflns_number_gt                2153
_reflns_number_total             2444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7019846-file003.cif
_cod_data_source_block           rh013
_cod_original_cell_volume        1983.63(17)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C37.50 H40.50 Cl2.50 N10 Ni2 O2'
_cod_database_code               4304486