Crystal structure of poly[(bis(isothiocyano)-bis(μ 2-(E)-N′-(pyridin-4-ylmethylene)isonicotinohydrazide))iron(II) – methanol – 1,4-dioxane (1/2/2), C36H44FeN10O8S2
Cui, Hong-Meng; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 801–803; doi:10.1515/ncrs-2022-0274

data_8107220
_publ_section_title
;
 Crystal structure of poly[(bis(isothiocyano)-bis(\m
 2-(E)-N&#x2032;-(pyridin-4-ylmethylene)isonicotinohydrazide))iron(II) --
 methanol -- 1,4-dioxane (1/2/2), C36H44FeN10O8S2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              801
_journal_page_last               803
_journal_paper_doi               10.1515/ncrs-2022-0274
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C26 H20 Fe N10 O2 S2, 2(C4 H8 O2), 2(C H4 O)'
_chemical_formula_sum            'C36 H44 Fe N10 O8 S2'
_chemical_formula_weight         864.78
_chemical_name_systematic
;
 <b>[catena-(bis(isothiocyano)-bis(\m~2~-(E)-N'-(pyridin-4-ylmethylene)\
isonicotinohydrazide))-iron(II)]-methanol(1/2)-(1,4-dioxane)(1/2)</b>
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 96.952(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7712(5)
_cell_length_b                   24.6087(12)
_cell_length_c                   9.6083(4)
_cell_measurement_reflns_used    2949
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.0091
_cell_measurement_theta_min      2.8602
_cell_volume                     2058.68(18)
_computing_cell_refinement       'CrysAlis^Pro^, Ver. 34.44 [1]'
_computing_data_collection       'CrysAlis^Pro^, Ver. 34.44 [1]'
_computing_data_reduction        'CrysAlis^Pro^, Ver. 34.44 [1]'
_computing_molecular_graphics    Mercury[5]
_computing_publication_material  Olex2[2]
_computing_structure_refinement  SHELXL[4]
_computing_structure_solution    'Olex2.solve [3]'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10617
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.073
_diffrn_reflns_theta_min         2.866
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.9490
_exptl_absorpt_correction_T_min  0.9490
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0413P)^2^+0.3724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3405
_reflns_number_total             4710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0274_suppl.cif
_cod_data_source_block           p
_cod_database_code               8107220
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.836
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-C17A \\sim O3-C17B
 with sigma of 0.02
 C16A-C17A \\sim C16A-C17B
 with sigma of 0.02
 O2-C16A \\sim O2-C16B
 with sigma of 0.02
 C16A-C17A \\sim C16B-C17A
 with sigma of 0.02
 C16A-C17B \\sim C16B-C17B
 with sigma of 0.02
 O2-C14A \\sim O2-C14B
 with sigma of 0.02
 C15A-C14A \\sim C15A-C14B
 with sigma of 0.02
 O3-C15A \\sim O3-C15B
 with sigma of 0.02
 C15A-C14A \\sim C15B-C14A
 with sigma of 0.02
 C15A-C14B \\sim C15B-C14B
 with sigma of 0.02
3. Others
 Sof(C17B)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(C16B)=Sof(H16C)=Sof(H16D)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(2)
 Sof(C14B)=Sof(H14C)=Sof(H14D)=1-FVAR(3)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=FVAR(3)
 Sof(C15B)=Sof(H15C)=Sof(H15D)=1-FVAR(4)
 Sof(C15A)=Sof(H15A)=Sof(H15B)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C14B(H14C,H14D), C15A(H15A,H15B), C15B(H15C,H15D), C16A(H16A,
 H16B), C16B(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              42679
_shelx_hkl_checksum              42071
_olex2_submission_special_instructions 'No special instructions were received'