Unusual Reactivity of Methylene Group Adjacent to Pyridine-2-Carboxamido Moiety in Iron(III) and Cobalt(III) Complexes
John M. Rowland; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 41 (2002) 2754–2760; doi:10.1021/ic011197e

data_4317982
_publ_section_title
;
 Unusual Reactivity of Methylene Group Adjacent to Pyridine-2-Carboxamido
 Moiety in Iron(III) and Cobalt(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2754
_journal_page_last               2760
_journal_paper_doi               10.1021/ic011197e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C25 H20 Cl Co N6 O9'
_chemical_formula_weight         642.85
_chemical_name_common            '[Co(bpca)~2~]ClO~4~^.^CH~3~OH'
_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                110.182(4)
_cell_angle_beta                 102.203(7)
_cell_angle_gamma                101.096(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8361(9)
_cell_length_b                   11.4944(12)
_cell_length_c                   14.4695(14)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.5
_cell_volume                     1290.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.10 (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL 6.10 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL 6.10 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17067
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         1.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     'omitted 0,0,1 due to extinction'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+1.0976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                6747
_reflns_number_total             7815
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic011197e_3.cif
_cod_data_source_block           mn1248
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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 
;
_cod_database_code               4317982