Bis[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]iron(III) perchlorate methanol solvate
Wu, Dayu; Acta Crystallographica Section E 65 (2009) m1340–; doi:10.1107/S1600536809040549

data_2224004
_publ_section_title
;
 Bis[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]iron(III)
 perchlorate methanol solvate
;
_journal_coeditor_code           SI2207
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1340
_journal_paper_doi               10.1107/S1600536809040549
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe (C12 H8 N3 O2)2] Cl O4, C H4 O'
_chemical_formula_moiety         'C24 H16 Fe N6 O4 +, Cl O4 -, C H4 O'
_chemical_formula_sum            'C25 H20 Cl Fe N6 O9'
_chemical_formula_weight         639.77
_chemical_name_systematic
;Bis[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]iron(III)
 perchlorate
methanol solvate
;
_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                109.507(4)
_cell_angle_beta                 103.394(3)
_cell_angle_gamma                100.091(3)
_cell_formula_units_Z            2
_cell_length_a                   8.799(3)
_cell_length_b                   11.603(4)
_cell_length_c                   14.356(6)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.787
_cell_measurement_theta_min      3.021
_cell_volume                     1292.0(8)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8499
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0537P)^2^+1.8601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                4177
_reflns_number_total             4421
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            si2207.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2224004
_cod_database_fobs_code          2224004