Tris(pyridinealdoximato)metal Complexes as Ligands for the Synthesis of Asymmetric Heterodinuclear CrIIIM Species [M = Zn(II), Cu(II), Ni(II), Fe(II), Mn(II), Cr(II), Co(III)]: A Magneto-Structural Study
Sylvia Ross; Thomas Weyhermüller; Eckhard Bill; Karl Wieghardt; Phalguni Chaudhuri; Inorganic Chemistry 40 (2001) 6656–6665; doi:10.1021/ic010552y

data_4320703
_publ_section_title
;
 Tris(pyridinealdoximato)metal Complexes as Ligands for the Synthesis of
 Asymmetric Heterodinuclear CrIIIM Species [M = Zn(II), Cu(II), Ni(II),
 Fe(II), Mn(II), Cr(II), Co(III)]: A Magneto-Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6656
_journal_page_last               6665
_journal_paper_doi               10.1021/ic010552y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     '[C27 H33 Cr N9 Ni O3 P]2+, 2(ClO4)-, H2O'
_chemical_formula_sum            'C27 H35 Cl2 Cr N9 Ni O12 P'
_chemical_formula_weight         890.22
_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                102.55(2)
_cell_angle_beta                 107.54(2)
_cell_angle_gamma                104.00(2)
_cell_formula_units_Z            2
_cell_length_a                   11.989(1)
_cell_length_b                   12.429(2)
_cell_length_c                   13.292(2)
_cell_measurement_reflns_used    6220
_cell_measurement_temperature    100(2)
_cell_volume                     1740.0(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'SIEMENS SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16913
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.69
_diffrn_standards_number         6220
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick, 1994'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1106
_refine_ls_wR_factor_obs         0.1007
_reflns_number_observed          6840
_reflns_number_total             9114
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010552y_5.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] 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^)+(0.0551P)^2^+0.0000P] 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        1740.0(4)
_cod_database_code               4320703