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_4320702
_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 H39 Cr Cu N9 O3]2+, 2 (ClO4)-'
_chemical_formula_sum            'C27 H39 Cl2 Cr Cu N9 O11'
_chemical_formula_weight         852.11
_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                111.74(3)
_cell_angle_beta                 102.04(3)
_cell_angle_gamma                101.77(3)
_cell_formula_units_Z            2
_cell_length_a                   12.063(2)
_cell_length_b                   12.627(3)
_cell_length_c                   12.910(3)
_cell_measurement_reflns_used    2915
_cell_measurement_temperature    100(2)
_cell_volume                     1698.6(9)
_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, 0.43 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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6826
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_correction_T_min  0.7956
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick, 1994'
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_obs          0.0588
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0089P)^2^+11.2869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1376
_refine_ls_wR_factor_obs         0.1138
_reflns_number_observed          3583
_reflns_number_total             4793
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010552y_4.cif
_cod_data_source_block           5
_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^)+(0.0089P)^2^+11.2869P] 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^)+(0.0089P)^2^+11.2869P] 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        1698.7(6)
_cod_database_code               4320702