Synthesis and Crystal Structure of the Bis(μ-hydroxo)diiron(II) Complex with Tridentate Ligands Having a Sterically Bulky Imidazolyl Group
Yaguchi, Reiko; Furutachi, Hideki; Shirotsuki, Sanae; Zhang, Xi; Ishikawa, Takanao; Akine, Shigehisa; Tosha, Takehiko; Fujinami, Shuhei; Suzuki, Masatatsu; Kitagawa, Teizo; X-ray Structure Analysis Online 35 (2019) 27–; doi:10.2116/xraystruct.35.27

data_1551063
_publ_section_title
;
 Synthesis and Crystal Structure of the Bis(\m-hydroxo)diiron(II) Complex
 with Tridentate Ligands Having a Sterically Bulky Imidazolyl Group
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              27
_journal_paper_doi               10.2116/xraystruct.35.27
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         C58H60Cl2Fe2N10O10
_chemical_formula_sum            'C58 H60 Cl2 Fe2 N10 O10'
_chemical_formula_weight         1239.76
_chemical_name_common            (C29H29N5)2Fe2(OH)2(ClO4)2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                63.254(12)
_cell_angle_beta                 86.458(19)
_cell_angle_gamma                79.581(17)
_cell_formula_units_Z            1
_cell_length_a                   11.007(2)
_cell_length_b                   11.5591(12)
_cell_length_c                   12.534(2)
_cell_measurement_reflns_used    15351
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.519
_cell_measurement_theta_min      2.647
_cell_volume                     1400.3(4)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measurement_device_type  'Rigaku Mercury (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15351
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.519
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            'pale yellow green'
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6735
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0447P)^2^+0.8254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6236
_reflns_number_total             6735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_27_1.txt
_cod_data_source_block           yaguti5
_cod_depositor_comments          'Fixing author names.'
_cod_original_cell_volume        1400.4(4)
_cod_database_code               1551063
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              57312
_shelx_hkl_checksum              21932