μ-Oxo-bis{[(6-hydroxymethyl-2-pyridylmethyl)bis(2-pyridylmethyl)amine-κ^5^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''',<i>O</i>]iron(III)} tetrakis(perchlorate)
Yun-Ling, Gao; Xiao-Jun, Peng; Shi-Guo, Sun; Chang-Neng, Chen; Li-Cheng, Sun; Acta Crystallographica Section C 61 (2005) m13–m15; doi:10.1107/S0108270104028148

data_2014597
_publ_section_title
;\m-Oxo-bis{[(6-hydroxymethyl-2-pyridylmethyl)bis(2-pyridylmethyl)amine-\k^5^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''',<i>O</i>]iron(III)}
 tetrakis(perchlorate)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m13
_journal_page_last               m15
_journal_paper_doi               10.1107/S0108270104028148
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe2 O (C19 H20 N4 O)2] (Cl O4)4'
_chemical_formula_moiety         'C38 H40 Fe2 N8 O3 4+, 4Cl O4 -'
_chemical_formula_sum            'C38 H40 Cl4 Fe2 N8 O19'
_chemical_formula_weight         1166.28
_chemical_name_systematic
;
\m-Oxo-bis{[(6-hydroxymethyl-2-pyridylmethyl)bis(2-pyridylmethyl)amine
-\k^5^N,N',N'',N''',O]iron(III)} tetrakis(perchlorate)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.220(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0733(9)
_cell_length_b                   9.9223(3)
_cell_length_c                   20.5055(8)
_cell_measurement_reflns_used    3348
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.81
_cell_volume                     4565.9(3)
_computing_cell_refinement       'SMART and SAINT (Siemens,1994)'
_computing_data_collection       'SMART (Siemens,1996)'
_computing_data_reduction        'SAINT? and XPREP in SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7191
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  .856
_exptl_absorpt_correction_T_min  .7128
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          .34
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.475
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0536P)^2^+58.9568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                3000
_reflns_number_total             4002
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1198.cif
_cod_data_source_block           I
_cod_depositor_comments
;
  Moved the _audit_creation_method data item out of the loop.

  Antanas Vaitkus,
  2019-03-01
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014597
_cod_database_fobs_code          2014597