Ethylene/propylene copolymerization catalyzed by half-titanocenes containing monodentate anionic nitrogen ligands: effect of ligands on catalytic behaviour and structure of copolymers
Zhang, Zhi-Qian; Qu, Jun-Teng; Zhang, Shu; Miao, Qiu-Ping; Wu, Yi-Xian; Polymer Chemistry 9 (2018) 48–; doi:10.1039/C7PY01807J

data_1548393
_publ_section_title
;
 Ethylene/propylene copolymerization catalyzed by half-titanocenes
 containing monodentate anionic nitrogen ligands: effect of ligands on
 catalytic behaviour and structure of copolymers
;
_journal_issue                   1
_journal_name_full               'Polymer Chemistry'
_journal_page_first              48
_journal_paper_doi               10.1039/C7PY01807J
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C32 H43 Cl2 N3 Ti, 0.5(C7 H8)'
_chemical_formula_sum            'C35.5 H47 Cl2 N3 Ti'
_chemical_formula_weight         634.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-14
_audit_creation_method
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.765(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.8611(10)
_cell_length_b                   19.4952(12)
_cell_length_c                   19.5123(11)
_cell_measurement_reflns_used    15854
_cell_measurement_temperature    106.1
_cell_measurement_theta_max      29.5231
_cell_measurement_theta_min      3.2366
_cell_volume                     6904.8(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      106.1
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -81.00  -39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222  -37.0000 -150.0000 42

  2 omega    9.00   35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222   77.0000  150.0000 26

  3 omega  -55.00    6.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222  -37.0000 -120.0000 61

  4 omega  -44.00   11.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222   93.0000   27.0000 55

  5 omega  -31.00   -5.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222  -93.0000  152.0000 26

  6 omega   28.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.5222   77.0000 -180.0000 25

  7 omega   -8.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8347  -93.0000  -83.0000 59

  8 omega  -46.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8347  -77.0000 -180.0000 86
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0175806000
_diffrn_orient_matrix_UB_12      -0.0298647000
_diffrn_orient_matrix_UB_13      0.0082084000
_diffrn_orient_matrix_UB_21      0.0033260000
_diffrn_orient_matrix_UB_22      -0.0157303000
_diffrn_orient_matrix_UB_23      -0.0317164000
_diffrn_orient_matrix_UB_31      0.0347261000
_diffrn_orient_matrix_UB_32      -0.0136196000
_diffrn_orient_matrix_UB_33      0.0187049000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50094
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         13543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+4.1401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                11265
_reflns_number_total             13543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7py01807j2.cif
_cod_data_source_block           exp_4900
_cod_depositor_comments
'Adding full bibliography for 1548391--1548393.cif.'
_cod_original_formula_sum        'C35.50 H47 Cl2 N3 Ti'
_cod_database_code               1548393
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32