Remarkably Robust Mono-n-butyl Group IV Dicyclohexylamido Complexes {(Cy)2N}3M(n-butyl) (Cy: cyclohexyl [C6H11], M: Ti, Zr)
Adler, Christian; Tomaschun, Gabriele; Schmidtmann, Marc; Beckhaus, Rüdiger; Organometallics 33 (2014) 7011–; doi:10.1021/om5008105

data_4085026
_publ_section_title
;
 Remarkably Robust Mono-n-butyl Group IV Dicyclohexylamido Complexes
 {(Cy)2N}3M(n-butyl) (Cy: cyclohexyl [C6H11], M: Ti, Zr)
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7011
_journal_paper_doi               10.1021/om5008105
_journal_volume                  33
_journal_year                    2014
_chemical_formula_structural     ZrCl(N(C6H11)2)3
_chemical_formula_sum            'C36 H66 Cl N3 Zr'
_chemical_formula_weight         667.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.5218(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7961(4)
_cell_length_b                   18.6744(7)
_cell_length_c                   39.6955(15)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.97
_cell_measurement_theta_min      2.24
_cell_volume                     7261.4(5)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            100222
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 8928 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         20603
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0300P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                19494
_reflns_number_total             20603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5008105_si_001.cif
_cod_data_source_block           (Cy2N)3ZrCl_(1b)
_cod_depositor_comments
'Adding full bibliography for 4085026--4085029.cif.'
_cod_database_code               4085026
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.938
_shelxl_version_number           2013-4
_shelx_res_checksum              36797