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_4335760
_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_formula_moiety         'C44 H22 F24 N8 Ni2 O1'
_chemical_formula_sum            'C44 H22 F24 N8 Ni2 O'
_chemical_formula_weight         1252.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-21
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 91.4730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1698(8)
_cell_length_b                   21.7745(16)
_cell_length_c                   19.0954(14)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     4642.8(6)
_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 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51146
_diffrn_reflns_theta_full        26.417
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         2.050
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.955
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488.000
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.52
_refine_diff_density_min         -1.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9567
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         13433
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.0047567
_refine_ls_shift/su_mean         0.0000769
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +14.92P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1974
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1974
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                8160
_reflns_number_total             13433
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.60
_oxford_diffrn_Wilson_scale      128.55
_oxford_refine_ls_r_factor_ref   0.1015
_oxford_refine_ls_scale          0.08510(3)
_oxford_reflns_number_all        13433
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10063_0m in P2(1)/c'
_cod_data_source_file            ic4011746_si_004.cif
_cod_data_source_block           10063
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C44 H22 F24 N8 Ni2 O1'
_cod_database_code               4335760