Redetermination of the crystal structure of bis(tri-2-pyridylamine)iron(II) bis(perchlorate), and a new refinement of the isotypic nickel(II) analogue: treatment of the perchlorate anion disorder
Setifi, Zouaoui; Setifi, Fatima; Dege, Necmi; El Ati, Rafika; Glidewell, Christopher; Acta Crystallographica Section E 74 (2018) 668–672; doi:10.1107/S2056989018005601

data_2242437
_publ_section_title
;
 Redetermination of the crystal structure of
 bis(tri-2-pyridylamine)iron(II) bis(perchlorate), and a new refinement of
 the isotypic nickel(II) analogue: treatment of the perchlorate anion
 disorder
;
_journal_coeditor_code           SU5436
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              668
_journal_page_last               672
_journal_paper_doi               10.1107/S2056989018005601
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe (C15 H12 N4)2] (Cl O4)2'
_chemical_formula_moiety         'C30 H24 Fe N8 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C30 H24 Cl2 Fe N8 O8'
_chemical_formula_weight         751.32
_chemical_name_systematic
;
Bis(tri-2-pyridylamine)iron(II) bis(perchlorate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.716(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3251(7)
_cell_length_b                   17.4731(11)
_cell_length_c                   11.0495(9)
_cell_measurement_reflns_used    3322
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.596
_cell_measurement_theta_min      2.199
_cell_volume                     1588.8(2)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
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_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.199
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED32; Stoe & Cie, 2002)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                2098
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5436sup1.cif
_cod_data_source_block           I
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_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.920
_shelx_hkl_checksum              67624
_shelx_res_checksum              69977
_shelxl_version_number           2.014
_cod_database_fobs_code 2242437