Titanium and zirconium complexes bearing new tridentate [OSO] bisphenolato-based ligands: synthesis, characterization and catalytic properties for alkene polymerization.
Song, Tingting; He, Jianghao; Liang, Liwei; Liu, Ning; Li, Feng; Tong, Xiaobo; Mu, Xiaoyue; Mu, Ying; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13719–13731; doi:10.1039/c9dt03225h

data_7700934
_publ_section_title
;
 Titanium and zirconium complexes bearing new tridentate [OSO]
 bisphenolato-based ligands: synthesis, characterization and catalytic
 properties for alkene polymerization.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13719
_journal_page_last               13731
_journal_paper_doi               10.1039/c9dt03225h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C44 H56 Cl2 O3 S Zr, 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H60 Cl6 O3 S Zr'
_chemical_formula_weight         996.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-08 deposited with the CCDC.    2019-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4804(4)
_cell_length_b                   25.1371(7)
_cell_length_c                   29.5376(7)
_cell_measurement_reflns_used    5851
_cell_measurement_temperature    173
_cell_measurement_theta_max      22.643
_cell_measurement_theta_min      2.253
_cell_volume                     10751.5(5)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            34750
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.036
_diffrn_reflns_theta_min         1.620
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+74.6340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4111
_reflns_number_total             5415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03225h2.cif
_cod_data_source_block           s_sq
_cod_depositor_comments
'Adding full bibliography for 7700933--7700935.cif.'
_cod_database_code               7700934
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C17, C18
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17, C19
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17, C20
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C17, C4
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              7068
_shelx_fab_checksum              43609
_olex2_submission_special_instructions 'No special instructions were received'