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_4333417
_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_analytical     '[C30 H42 N9 Ni2 O3 ]+, (CLO4)-, 0.5 CH3OH'
_chemical_formula_sum            'C30.5 H44 Cl N9 Ni2 O7.5'
_chemical_formula_weight         809.62
_chemical_name_systematic
;
  ?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                119.548(3)
_cell_angle_beta                 101.498(3)
_cell_angle_gamma                102.176(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6289(4)
_cell_length_b                   13.8230(5)
_cell_length_c                   13.8607(5)
_cell_measurement_reflns_used    59715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.04
_cell_measurement_theta_min      2.91
_cell_volume                     1770.03(14)
_computing_cell_refinement       'BRUKER AXS Collect Software'
_computing_data_collection       'BRUKER AXS Collect Software'
_computing_data_reduction        'BRUKER AXS Collect Software'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method
'800 images at 1 deg. stepwise rotation in omega and phi, 10 sec./ frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34026
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.061
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         10284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_obs          0.0289
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+1.3372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0722
_refine_ls_wR_factor_obs         0.0708
_reflns_number_observed          9630
_reflns_number_total             10289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic701073jsup1.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0260P)^2^+1.3372P] 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^)+(0.0260P)^2^+1.3372P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1770.03(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.50 H44 Cl N9 Ni2 O7.50'
_cod_database_code               4333417