Synthesis and Characterization of Group 4 Amidinate Amide Complexes M[CyNC(Me)NCy]2(NR2)2(R = Me, M = Ti, Zr, Hf; R = Et, M = Zr)
Sun, Jia-Feng; Chen, Shu-Jian; Duan, Yuxi; Li, Yi-Zhi; Chen, Xue-Tai; Xue, Zi-Ling; Organometallics 28 (2009) 3088–; doi:10.1021/om900162b

data_4069375
_publ_section_title
;
 Synthesis and Characterization of Group 4 Amidinate Amide Complexes
 M[CyNC(Me)NCy]2(NR2)2(R = Me, M = Ti, Zr, Hf; R = Et, M = Zr)
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3088
_journal_paper_doi               10.1021/om900162b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C32 H62 N6 Ti'
_chemical_formula_sum            'C32 H62 N6 Ti'
_chemical_formula_weight         578.78
_chemical_name_common            'Amino Titanium'
_chemical_name_systematic
; 
 Amino Titanium 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.415(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.522(5)
_cell_length_b                   9.264(4)
_cell_length_c                   18.163(8)
_cell_measurement_temperature    163(2)
_cell_volume                     1714.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10522
_diffrn_reflns_theta_full        20.20
_diffrn_reflns_theta_max         20.20
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.9465
_exptl_absorpt_correction_T_min  0.9212
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.129
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.73(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.502
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.502
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1199P)^2^+4.1008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                3216
_reflns_number_total             3271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900162b_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1714.9(14)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4069375