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_4335759
_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         'C32.50 H21 Cl1.00 F12 N6 Ni1 O2'
_chemical_formula_sum            'C32.5 H21 Cl F12 N6 Ni O2'
_chemical_formula_weight         849.70
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-07-15
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                99.4930(10)
_cell_angle_beta                 102.1210(10)
_cell_angle_gamma                105.6180(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0789(4)
_cell_length_b                   11.1534(5)
_cell_length_c                   18.2342(8)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1689.82(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.025
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52114
_diffrn_reflns_theta_full        29.632
_diffrn_reflns_theta_max         30.236
_diffrn_reflns_theta_min         1.175
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       prism
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.759
_exptl_crystal_size_mid          0.536
_exptl_crystal_size_min          0.354
_refine_diff_density_max         1.90
_refine_diff_density_min         -1.01
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9924
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9998
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.0045803
_refine_ls_shift/su_mean         0.0001656
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 2.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1099
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1099
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                9648
_reflns_number_total             9998
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.76
_oxford_diffrn_Wilson_scale      46.09
_oxford_refine_ls_r_factor_ref   0.0412
_oxford_refine_ls_scale          0.14521(5)
_oxford_reflns_number_all        9998
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'mo_10062_0m in P-1'
_cod_data_source_file            ic4011746_si_003.cif
_cod_data_source_block           10062
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C32.50 H21 Cl1.00 F12 N6 Ni1 O2'
_cod_database_code               4335759