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_4317981
_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            'C24 H20 B Cl0 F4 Fe N6 O2'
_chemical_formula_weight         567.12
_chemical_name_common            '[Fe(pmp)2]BF4'
_chemical_name_systematic
;

  ?

;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.972(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6168(16)
_cell_length_b                   8.8823(16)
_cell_length_c                   15.505(3)
_cell_measurement_reflns_used    675
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.5
_cell_volume                     1168.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.088
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10616
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.7953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                4861
_reflns_number_total             6356
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic011197e_2.cif
_cod_data_source_block           mn1256
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4317981