Zwitterionic d0Metal Complexes [(Cy2N)3M]+[(μ-Me)B(C6F5)3]−(M = Ti, Zr, Hf) Derived from Tris(dicyclohexylamido)methyl Metal Precursors
Adler, Christian; Frerichs, Nils; Schmidtmann, Marc; Beckhaus, Rüdiger; Organometallics 35 (2016) 3728–; doi:10.1021/acs.organomet.6b00688

data_4089069
_publ_section_title
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 Zwitterionic d0Metal Complexes [(Cy2N)3M]+[(\m-Me)B(C6F5)3]&#x2212;(M =
 Ti, Zr, Hf) Derived from Tris(dicyclohexylamido)methyl Metal Precursors
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_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3728
_journal_paper_doi               10.1021/acs.organomet.6b00688
_journal_volume                  35
_journal_year                    2016
_chemical_formula_structural     '[Ti(N(C6H11)2)3] [B(CH3)(C6F5)3] *2.5C7H8'
_chemical_formula_sum            'C72.5 H89 B F15 N3 Ti'
_chemical_formula_weight         1346.17
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.9270(4)
_cell_length_b                   16.9270(4)
_cell_length_c                   39.8167(12)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.41
_cell_volume                     9880.0(4)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0500
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            69469
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.026
_diffrn_reflns_theta_min         1.480
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             4242
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4840
_reflns_number_total             6420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00688_si_002.cif
_cod_data_source_block           '[(Cy2N)3Ti][MeB(C6F5)3_(3-Ti)'
_cod_original_cell_volume        9879.9(5)
_cod_original_formula_sum        'C72.50 H89 B F15 N3 Ti'
_cod_database_code               4089069
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              79516
_shelx_hkl_checksum              22059