Synthesis of Ti, Zr, and Hf complexes with a new tetra-azane ligand by one-pot HCl-elimination and their properties as catalysts for production of UHMWPE
Ji, Xiangdong; Yao, Wei; Luo, Xuyang; Gao, Wei; Mu, Ying; New J. Chem. 40 (2016) 2071–; doi:10.1039/C5NJ02151K

data_7055244
_publ_section_title
;
 Synthesis of Ti, Zr, and Hf complexes with a new tetra-azane ligand by
 one-pot HCl-elimination and their properties as catalysts for production
 of UHMWPE
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2071
_journal_paper_doi               10.1039/C5NJ02151K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C44.5 H49 Cl3 N4 Ti'
_chemical_formula_weight         794.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-01 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                100.5720(10)
_cell_angle_beta                 101.7320(10)
_cell_angle_gamma                104.8770(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7714(8)
_cell_length_b                   11.1493(8)
_cell_length_c                   19.3176(14)
_cell_measurement_reflns_used    3158
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.22
_cell_volume                     2126.1(3)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0227
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11488
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.9161
_exptl_absorpt_correction_T_min  0.8976
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+1.1596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                6414
_reflns_number_total             8188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02151k2.cif
_cod_data_source_block           Complex_1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055242--7055246.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C44.50 H49 Cl3 N4 Ti'
_cod_database_code               7055244