Six-coordinate CoIII and four-coordinate MII (M = Co, Zn) mixed-valence dimers supported by a deprotonated pyridine amide ligand: magnetism of a CoIIICoII complex and C‒H⋯O/Cl/Br interactions
Jacob, Wilson; Mishra, Haritosh; Pandey, Sharmila; Lloret, Francesc; Mukherjee, Rabindranath; New Journal of Chemistry 33 (2009) 893–; doi:10.1039/b814303j

data_7051621
_publ_section_title
;
 Six-coordinate CoIII and four-coordinate MII (M = Co, Zn)
 mixed-valence dimers supported by a deprotonated pyridine amide
 ligand: magnetism of a CoIIICoII complex and C--H&#x22EF;O/Cl/Br
 interactions
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              893
_journal_paper_doi               10.1039/b814303j
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C37 H44 Cl2 Co N9 O9 Zn'
_chemical_formula_sum            'C37 H44 Cl2 Co N9 O9 Zn'
_chemical_formula_weight         954.02
_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-97
_cell_angle_alpha                78.089(5)
_cell_angle_beta                 72.040(5)
_cell_angle_gamma                86.649(5)
_cell_formula_units_Z            2
_cell_length_a                   11.555(5)
_cell_length_b                   12.482(5)
_cell_length_c                   16.117(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.35
_cell_volume                     2163.6(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1641
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10253
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.9795
_exptl_absorpt_correction_T_min  0.9031
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.46
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The data-set of 3 was treated with the SQUEEZE filter due to
the presence of severely disordered solvent molecules and counter
anion which could not be modeled satisfactorily. The SQUEEZE process
reported that the disordered solvent and chloride components accounted
for 171 electrons per unit cell or half that number that is 85.5 (one
methanol, five water and one chloride) per cation in a volume of 571.0
\%A3 out of a unit volume of 2163.6 \%A3. These disordered molecules were
included in the final chemical formula (Table 4). The values of f(000),
Dcalc, M and Mu have been calculated on this assumption.
;
_refine_diff_density_max         1.764
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2691
_reflns_number_gt                4663
_reflns_number_total             10253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814303j.txt
_cod_data_source_block           dec19sq
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051621