Crystal structure of bis(2-methoxy-6-((2-(pyrimidin-2-yl)hydrazono)methyl)phenolato-κ3 N,N′,O)iron(III) perchlorate, C24H22N8O8ClFe
Song, Jun-Ying; Wang, Zi-Chuang; Zhang, Juan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 133–135; doi:10.1515/ncrs-2018-0227

data_8105566
_publ_section_title
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 Crystal structure of
 bis(2-methoxy-6-((2-(pyrimidin-2-yl)hydrazono)methyl)phenolato-\k3
 N,N&#x2032;,O)iron(III) perchlorate, C24H22N8O8ClFe
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_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              133
_journal_page_last               135
_journal_paper_doi               10.1515/ncrs-2018-0227
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C24 H22 Fe N8 O4, Cl O4'
_chemical_formula_sum            'C24 H22 Cl Fe N8 O8'
_chemical_formula_weight         641.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                82.119(4)
_cell_angle_beta                 83.277(4)
_cell_angle_gamma                87.206(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4568(4)
_cell_length_b                   10.5977(4)
_cell_length_c                   12.0793(6)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.4210
_cell_measurement_theta_min      3.6960
_cell_volume                     1316.12(10)
_computing_cell_refinement       'CrysAlis^Pro^ [1]'
_computing_data_collection       'CrysAlis^Pro^ [1]'
_computing_data_reduction        'CrysAlis^Pro^ [1]'
_computing_molecular_graphics    'Olex2 [2]'
_computing_publication_material  'Olex2 [2]'
_computing_structure_refinement  'ShelXL-2015 [3]'
_computing_structure_solution    'ShelXS-2008 [4]'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8616
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.996
_diffrn_reflns_theta_min         11.216
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.113
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47390
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       cube
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^+0.5668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4310
_reflns_number_total             4936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0227_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1316.11(9)
_cod_database_code               8105566
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N7(H7), C1(H1), C2(H2), C3(H3A), C5(H5), C7(H7A), C8(H8), C9(H9),
 C13(H13), C14(H14), C15(H15), C17(H17), C19(H19), C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C24(H24A,H24B,H24C)
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