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_4340889
_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            'C44 H46 B Fe3 N6 O S Tl'
_chemical_formula_weight         1089.66
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                71.3780(10)
_cell_angle_beta                 77.6110(10)
_cell_angle_gamma                71.2460(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5633(7)
_cell_length_b                   13.6431(8)
_cell_length_c                   14.3940(9)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.51
_cell_volume                     2021.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         1.505
_exptl_absorpt_coefficient_mu    5.124
_exptl_absorpt_correction_T_max  0.7318
_exptl_absorpt_correction_T_min  0.2025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         9228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.5299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8796
_reflns_number_total             9228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5015658_si_002.cif
_cod_data_source_block           kla0244
_cod_depositor_comments
'Adding full bibliography for 4340887--4340894.cif.'
_cod_database_code               4340889
_shelx_estimated_absorpt_t_min   0.202
_shelx_estimated_absorpt_t_max   0.732
_shelxl_version_number           2013-4
_shelx_res_checksum              6852
_shelx_hkl_checksum              65337