Crystal Structure of μ-Phenoxo-μ-benzoate-bridged Dinuclear Fe(II) Complex with a Dinucleating Ligand Having a Sterically Bulky Imidazolyl Group
YASUDA, Yuichi; FURUTACHI, Hideki; HAYASHI, Yosuke; ISHIZAKI, Kana; FUJINAMI, Shuhei; AKINE, Shigehisa; SUZUKI, Masatatsu; NAGATOMO, Shigenori; KITAGAWA, Teizo; X-ray Structure Analysis Online 35 (2019) 11–; doi:10.2116/xraystruct.35.11

data_1551536
_publ_section_title
;
 Crystal Structure of \m-Phenoxo-\m-benzoate-bridged Dinuclear Fe(II)
 Complex with a Dinucleating Ligand Having a Sterically Bulky Imidazolyl
 Group
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              11
_journal_paper_doi               10.2116/xraystruct.35.11
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         C96H101B2F8Fe2N13O6
_chemical_formula_sum            'C96 H101 B2 F8 Fe2 N13 O6'
_chemical_formula_weight         1818.21
_chemical_name_common            '[LFe2(PhCO2)(MeCN)](BF4)2_2MeCN_3EtOH'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.3460(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5690(10)
_cell_length_b                   23.8260(8)
_cell_length_c                   24.821(2)
_cell_measurement_reflns_used    42650
_cell_measurement_temperature    108
_cell_measurement_theta_max      27.484
_cell_measurement_theta_min      2.362
_cell_volume                     9167.2(10)
_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    'SIR-92 (Altomare, et al., 1992)'
_diffrn_ambient_temperature      108
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_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  0.0207
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42650
_diffrn_reflns_point_group_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.362
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 5986 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1482
_refine_ls_number_reflns         16812
_refine_ls_number_restraints     623
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0221P)^2^+7.4251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.623
_reflns_number_gt                15982
_reflns_number_total             16812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_11_1.txt
_cod_data_source_block           yasu49
_cod_database_code               1551536
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              96146
_shelx_hkl_checksum              28121