Tridentate Facial Ligation of Tris(pyridine-2-aldoximato)nickel(II) and Tris(imidazole-2-aldoximato)nickel(II) To Generate NiIIFeIIINiII, MnIIINiII, NiIINiII, and ZnIINiIIand the Electrooxidized MnIVNiII, NiIINiIII, and ZnIINiIIISpecies: A Magnetostructural, Electrochemical, and EPR Spectroscopic Study
Chaudhuri, Phalguni; Weyhermüller, Thomas; Wagner, Rita; Khanra, Sumit; Biswas, Biplab; Bothe, Eberhard; Bill, Eckhard; Inorganic Chemistry 46 (2007) 9003–9016; doi:10.1021/ic701073j

data_4333415
_publ_section_title
;
 Tridentate Facial Ligation of Tris(pyridine-2-aldoximato)nickel(II) and
 Tris(imidazole-2-aldoximato)nickel(II) To Generate NiIIFeIIINiII,
 MnIIINiII, NiIINiII, and ZnIINiIIand the Electrooxidized MnIVNiII,
 NiIINiIII, and ZnIINiIIISpecies:&#x00A0; A Magnetostructural,
 Electrochemical, and EPR Spectroscopic Study
;
_journal_issue                   21
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9003
_journal_page_last               9016
_journal_paper_doi               10.1021/ic701073j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[C27 H36 Mn N9 Ni O3]2+, 2 (Cl O4)-, MeCN'
_chemical_formula_sum            'C29 H39 Cl2 Mn N10 Ni O11'
_chemical_formula_weight         888.25
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.73(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.9574(7)
_cell_length_b                   24.6226(9)
_cell_length_c                   14.9959(6)
_cell_measurement_temperature    100(2)
_cell_volume                     7368.4(5)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method
'1028 images at 1.0 deg. stepwise rotation in omega and phi, 210 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            103950
_diffrn_reflns_theta_full        30.97
_diffrn_reflns_theta_max         30.97
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+23.4182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                8284
_reflns_number_total             11701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701073jsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+23.4182P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+23.4182P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4333415