Synthesis and Oxidative Reactivity of 2,2'-Pyridylpyrrolide Complexes of Ni(II)
Nikolay P. Tsvetkov; Chun-Hsing Chen; José G. Andino; Richard L. Lord; Maren Pink; René W. Buell; Kenneth G. Caulton; Inorganic Chemistry 52 (2013) 9511–9521; doi:10.1021/ic4011746

data_4335761
_publ_section_title
;
 Synthesis and Oxidative Reactivity of 2,2'-Pyridylpyrrolide Complexes of
 Ni(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9511
_journal_page_last               9521
_journal_paper_doi               10.1021/ic4011746
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H10 Br4 F12 N4 Ni1'
_chemical_formula_sum            'C22 H10 Br4 F12 N4 Ni'
_chemical_formula_weight         936.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-07-01
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 111.838(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1424(11)
_cell_length_b                   13.8621(14)
_cell_length_c                   10.6833(11)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1394.2(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16010
_diffrn_reflns_theta_full        30.054
_diffrn_reflns_theta_max         30.054
_diffrn_reflns_theta_min         2.054
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.531
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   'USER DEFINED ABSORPTION METHOD'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0001
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7868
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.0138035
_refine_ls_shift/su_mean         0.0003899
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 2.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1091
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1091
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -18
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                6251
_reflns_number_total             7868
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.43
_oxford_diffrn_Wilson_scale      59.10
_oxford_refine_ls_r_factor_ref   0.0613
_oxford_refine_ls_scale          0.13005(4)
_oxford_reflns_number_all        7868
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10064_0m in P2(1)'
_cod_data_source_file            ic4011746_si_005.cif
_cod_data_source_block           10064
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C22 H10 Br4 F12 N4 Ni1'
_cod_database_code               4335761