Synthesis, characterization and olefin polymerization behaviors of phenylene-bridged bis-β-carbonylenamine binuclear titanium complexes
Luo, Derong; Zeng, Yi; Chen, Xiong; Xia, Ping; Xie, Guangyong; You, Qingliang; Zhang, Li; Li, Tingcheng; Li, Xiangdan; Zhang, Aiqing; RSC Advances 8 (2018) 6954–; doi:10.1039/C8RA00071A

data_7230150
_publ_section_title
;
 Synthesis, characterization and olefin polymerization behaviors of
 phenylene-bridged bis-\b-carbonylenamine binuclear titanium complexes
;
_journal_issue                   13
_journal_name_full               'RSC Advances'
_journal_page_first              6954
_journal_paper_doi               10.1039/C8RA00071A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C38 H48 N2 O2 S2'
_chemical_formula_sum            'C38 H48 N2 O2 S2'
_chemical_formula_weight         628.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-11-22 deposited with the CCDC.
2018-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.710(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.149(5)
_cell_length_b                   10.258(3)
_cell_length_c                   24.194(8)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    130
_cell_measurement_theta_max      19.209
_cell_measurement_theta_min      2.360
_cell_volume                     3487(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1731
_diffrn_reflns_av_unetI/netI     0.1690
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22094
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         1.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0853 before and 0.0728 after correction.
The Ratio of minimum to maximum transmission is 0.7967.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0916
_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^)+(0.1328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2702
_reflns_number_total             6060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra00071a1.cif
_cod_data_source_block           mo_dm15363_0m
_cod_original_cell_volume        3487.7(19)
_cod_database_code               7230150
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C36(H36A,H36B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C4(H4), C5(H5), C11(H11), C18(H18), C19(H19),
  C20(H20), C22(H22), C24(H24), C31(H31), C32(H32), C33(H33), C34(H34)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              37129
_olex2_submission_special_instructions 'No special instructions were received'