Bis(μ-{(1,3-phenylene)[<i>tert</i>-butyl(pyrazol-1-yl)borato][<i>tert</i>-butyl(dipyrazol-1-yl)borato]})dihydroxydiiron(II) tetrahydrofuran disolvate
Zhang, Fan; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 63 (2007) m2505–m2505; doi:10.1107/S1600536807043346

data_2215327
_publ_section_title
;Bis(\m-{(1,3-phenylene)[<i>tert</i>-butyl(pyrazol-1-yl)borato][<i>tert</i>-butyl(dipyrazol-1-yl)borato]})dihydroxydiiron(II)
 tetrahydrofuran disolvate
;
_journal_coeditor_code           AT2388
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2505
_journal_page_last               m2505
_journal_paper_doi               10.1107/S1600536807043346
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Fe2 (C23 H32 B2 N6 O)2], 2C4 H8 O'
_chemical_formula_moiety         'C46 H64 B4 Fe2 N12 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C54 H80 B4 Fe2 N12 O4'
_chemical_formula_weight         1116.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.619(12)
_cell_angle_beta                 63.139(12)
_cell_angle_gamma                66.862(13)
_cell_formula_units_Z            1
_cell_length_a                   11.645(2)
_cell_length_b                   12.363(2)
_cell_length_c                   12.507(2)
_cell_measurement_reflns_used    10281
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      3.4
_cell_volume                     1456.1(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
'SHELXL97 (Sheldrick, 1997) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE IPDS II two-circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12022
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9317
_exptl_absorpt_correction_T_min  0.8431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0841P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1548
_reflns_number_gt                3411
_reflns_number_total             5438
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2388.cif
_cod_data_source_block           I
_cod_database_code               2215327
_cod_database_fobs_code          2215327