Ferrocenyl-Substituted Tris(pyrazolyl)borates-A New Ligand Type Combining Redox Activity with Resistance to Hydrogen Atom Abstraction.
Sirianni, Eric R.; Yap, Glenn P. A.; Theopold, Klaus H.; Inorganic chemistry 53 (2014) 9424–9430; doi:10.1021/ic5015658

data_4340892
_publ_section_title
;
 Ferrocenyl-Substituted Tris(pyrazolyl)borates-A New Ligand Type Combining
 Redox Activity with Resistance to Hydrogen Atom Abstraction.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9424
_journal_page_last               9430
_journal_paper_doi               10.1021/ic5015658
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C45 H38 B Fe3 N6 Tl'
_chemical_formula_weight         1045.54
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.011(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8746(14)
_cell_length_b                   13.8172(17)
_cell_length_c                   23.992(3)
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    200(2)
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_cell_volume                     3850.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         1.753
_exptl_absorpt_coefficient_mu    5.323
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8790
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0294P)^2^+0.2251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6866
_reflns_number_total             8790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5015658_si_002.cif
_cod_data_source_block           kla0030
_cod_depositor_comments
'Adding full bibliography for 4340887--4340894.cif.'
_cod_database_code               4340892
_shelx_estimated_absorpt_t_min   0.268
_shelx_estimated_absorpt_t_max   0.438
_shelxl_version_number           2013-4
_shelx_res_checksum              61438
_shelx_hkl_checksum              85277