Crystal Structure of Bis(μ-hydroxo)diiron(III) Complex with Tripodal Ligands Having a Terminal Carboxylate Group
ZHANG, Xi; FURUTACHI, Hideki; OHYAMA, Yuya; FUJINAMI, Shuhei; AKINE, Shigehisa; SUZUKI, Masatatsu; X-ray Structure Analysis Online 35 (2019) 17–; doi:10.2116/xraystruct.35.17

data_1551528
_publ_section_title
;
 Crystal Structure of Bis(\m-hydroxo)diiron(III) Complex with Tripodal
 Ligands Having a Terminal Carboxylate Group
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              17
_journal_paper_doi               10.2116/xraystruct.35.17
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         C34H58Br0.04Fe2N7.96O19.87
_chemical_formula_sum            'C34 H58 Br0.04 Fe2 N7.96 O19.87'
_chemical_formula_weight         1011.38
_chemical_name_common            C17H20N3O2)2Fe2(OH)2(NO3)1.9553Br0.0447(H2O)8
_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                82.119(10)
_cell_angle_beta                 85.340(10)
_cell_angle_gamma                68.871(7)
_cell_formula_units_Z            2
_cell_length_a                   10.3845(15)
_cell_length_b                   11.1976(15)
_cell_length_c                   20.389(4)
_cell_measurement_reflns_used    23558
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.483
_cell_measurement_theta_min      3.028
_cell_volume                     2189.3(6)
_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 0.970
_diffrn_measured_fraction_theta_max 0.954
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23558
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7699
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_17_1.txt
_cod_data_source_block           f21
_cod_database_code               1551528
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.743
_shelx_estimated_absorpt_t_max   0.858
_shelx_res_checksum              22166
_shelx_hkl_checksum              17657