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_4340894
_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            'C42 H40 B Fe3 N6 Tl'
_chemical_formula_weight         1011.53
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                108.3310(10)
_cell_angle_beta                 106.4350(10)
_cell_angle_gamma                109.8410(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0542(7)
_cell_length_b                   13.1951(7)
_cell_length_c                   13.3690(7)
_cell_measurement_reflns_used    6542
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.63
_cell_volume                     1850.07(17)
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24505
_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         27.511
_diffrn_reflns_theta_min         1.783
_exptl_absorpt_coefficient_mu    5.535
_exptl_absorpt_correction_T_max  0.7324
_exptl_absorpt_correction_T_min  0.4408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0301P)^2^+0.2560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7471
_reflns_number_total             8491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5015658_si_002.cif
_cod_data_source_block           kla0243
_cod_depositor_comments
'Adding full bibliography for 4340887--4340894.cif.'
_cod_database_code               4340894
_shelx_estimated_absorpt_t_min   0.441
_shelx_estimated_absorpt_t_max   0.732
_shelxl_version_number           2013-4
_shelx_res_checksum              98203
_shelx_hkl_checksum              26910