μ-Oxo-bis(μ-2-furancarboxylato)bis{[<i>N</i>-methyl-<i>N</i>,<i>N</i>-bis(2-pyridylmethyl)amine]iron(III)} bis(perchlorate) methanol solvate
Nielsen, Anne.; Bond, Andrew D.; McKenzie, Christine J.; Acta Crystallographica Section E 60 (2004) m1959–m1960; doi:10.1107/S1600536804030375

data_2204725
_publ_section_title
;\m-Oxo-bis(\m-2-furancarboxylato)bis{[<i>N</i>-methyl-<i>N</i>,<i>N</i>-bis(2-pyridylmethyl)amine]iron(III)}
 bis(perchlorate) methanol solvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1959
_journal_page_last               m1960
_journal_paper_doi               10.1107/S1600536804030375
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[C36 H36 Fe2 N6 O7 2] (Cl O4)2 , C H4 O'
_chemical_formula_moiety         'C36 H36 Fe2 N6 O7 2+, 2(Cl O4 -), C H4 O'
_chemical_formula_sum            'C37 H40 Cl2 Fe2 N6 O16'
_chemical_formula_weight         1007.35
_chemical_name_systematic
;
 \m-oxo-bis(\m-2-furancarboxylato)bis(N-methyl-N,N-bis(2-pyridylmethyl)amine)
 diiron(III) bis(perchlorate) methanol solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.2770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1111(6)
_cell_length_b                   13.7316(5)
_cell_length_c                   20.1356(10)
_cell_measurement_reflns_used    5148
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.51
_cell_volume                     4151.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w and \f scans'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24686
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.698
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+6.5832P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                3740
_reflns_number_total             5149
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6012.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2204725
_cod_database_fobs_code          2204725