Crystal Structure of Bis(μ-hydroxo)diiron(II) Complex with a Dinucleating Ligand Having a Butyl Linker
SEKINO, Mio; FURUTACHI, Hideki; TASAKI, Kyosuke; ISHIKAWA, Takanao; FUJINAMI, Shuhei; AKINE, Shigehisa; SAKATA, Yoko; SUZUKI, Masatatsu; NOMURA, Takashi; OGURA, Takashi; KITAGAWA, Teizo; X-ray Structure Analysis Online 35 (2019) 5–; doi:10.2116/xraystruct.35.5

data_1551535
_publ_section_title
;
 Crystal Structure of Bis(\m-hydroxo)diiron(II) Complex with a
 Dinucleating Ligand Having a Butyl Linker
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              5
_journal_paper_doi               10.2116/xraystruct.35.5
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         C85.60H94.20B2Fe2N6O3.70
_chemical_formula_sum            'C85.6 H94.2 B2 Fe2 N6 O3.7'
_chemical_formula_weight         1399.58
_chemical_name_common            (C32H40N6)Fe2(OH)2(BPh4)2(Me2CO)1.2(Et2O)0.5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.522(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.678(3)
_cell_length_b                   16.3791(16)
_cell_length_c                   22.447(3)
_cell_measurement_reflns_used    31400
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.476
_cell_measurement_theta_min      3.084
_cell_volume                     7414.5(16)
_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      93
_diffrn_detector_area_resol_mean 14.4613
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79258
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.084
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2966
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         16779
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0573P)^2^+5.2583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14664
_reflns_number_total             16779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_5_2.txt
_cod_data_source_block           sekino4
_cod_original_cell_volume        7414.5(14)
_cod_original_formula_sum        'C85.60 H94.20 B2 Fe2 N6 O3.70'
_cod_database_code               1551535
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              89545
_shelx_hkl_checksum              10069