A rare octacoordinated mononuclear iron(III) spin-crossover compound: synthesis, crystal structure and magnetic properties
Hao, Xiaoyun; Cao, Tong; Dou, Yong; Yang, Lu; Zhou, Zhen; Zhang, Daopeng; Hao, Hongguo; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620010451

data_2022217
_publ_section_title
;
 A rare octacoordinated mononuclear iron(III) spin-crossover compound:
 synthesis, crystal structure and magnetic properties
;
_journal_coeditor_code           LF3118
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620010451
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'(C16 H36 N) [Fe (C12 H6 N10)2], 0.5C H4 O, 2H2 O1'
_chemical_formula_moiety
'C16 H36 N +, C24 H12 Fe1 N20 -, 0.5C H4 O, 2H2 O1'
_chemical_formula_sum            'C40.5 H54 Fe N21 O2.5'
_chemical_formula_weight         930.80
_chemical_name_systematic
;
Tetra-<i>n</i>-butylammonium
bis[6,6'-bis(tetrazol-1-id-5-yl)-2,2'-bipyridine]iron(III)
methanol hemisolvate dihydrate
;
_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   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                84.538(8)
_cell_angle_beta                 86.265(7)
_cell_angle_gamma                85.919(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5006(10)
_cell_length_b                   12.7609(10)
_cell_length_c                   15.0775(16)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0080
_cell_measurement_theta_min      3.0239
_cell_volume                     2384.0(4)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2001)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2001)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15117
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.282
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.557
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8320
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0894P)^2^+2.2058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1664
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                6081
_reflns_number_total             8320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3118sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C40.5 H54 Fe1 N21 O2.5'
_cod_database_code               2022217
_shelx_estimated_absorpt_t_min   0.918
_shelx_estimated_absorpt_t_max   0.960
_shelx_hkl_checksum              25764
_shelx_res_checksum              6398
_cod_database_fobs_code 2022217