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_4089070
_publ_section_title
;
 Zwitterionic d0Metal Complexes [(Cy2N)3M]+[(\m-Me)B(C6F5)3]&#x2212;(M =
 Ti, Zr, Hf) Derived from Tris(dicyclohexylamido)methyl Metal Precursors
;
_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_absolute_configuration ad
_chemical_formula_structural     '[Zr(N(C6H11)2)3] [B(CH3)(C6F5)3]'
_chemical_formula_sum            'C55 H69 B F15 N3 Zr'
_chemical_formula_weight         1159.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   25.1423(8)
_cell_length_b                   12.1416(4)
_cell_length_c                   17.4552(6)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.58
_cell_measurement_theta_min      2.20
_cell_volume                     5328.5(3)
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60344
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         1.620
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 3343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         10057
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                8241
_reflns_number_total             10057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00688_si_002.cif
_cod_data_source_block           '[(Cy2N)3Zr][MeB(C6F5)3_(3-Zr)'
_cod_database_code               4089070
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              51831
_shelx_hkl_checksum              25870