Ti and Zr complexes bearing guanidine-phenolate ligands: coordination chemistry and polymerization studies
Flores-Romero, Víctor; LeBlanc, Jesse; Chen, Zichuan; Lavoie, Gino G.; RSC Advances 14 (2024) 25889–25899; doi:10.1039/D4RA05146G

data_7249224
_publ_section_title
;
 Ti and Zr complexes bearing guanidine-phenolate ligands: coordination
 chemistry and polymerization studies
;
_journal_issue                   35
_journal_name_full               'RSC Advances'
_journal_page_first              25889
_journal_page_last               25899
_journal_paper_doi               10.1039/D4RA05146G
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C30 H40 Cl2 N6 O2 Ti, C7 H8'
_chemical_formula_sum            'C37 H48 Cl2 N6 O2 Ti'
_chemical_formula_weight         727.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.817(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6343(7)
_cell_length_b                   30.9675(18)
_cell_length_c                   12.5823(8)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.04
_cell_measurement_theta_min      2.26
_cell_volume                     3873.1(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            150839
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.152
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       rod
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         11792
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0494P)^2^+2.5209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10282
_reflns_number_total             11792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05146g2.cif
_cod_data_source_block           vfr31_exfs_a
_cod_database_code               7249224
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6S-C1S \\sim C9S-C8S
 with sigma of 0.02
 C6S-C5S \\sim C9S-C10S
 with sigma of 0.02
 C2S-C3S \\sim C13S-C12S
 with sigma of 0.02
 C1S-C7S \\sim C8S-C14S
 with sigma of 0.02
 C6S-C7S \\sim C9S-C14S
 with sigma of 0.04
 C1S-C5S \\sim C8S-C10S
 with sigma of 0.04
3. Others
 Sof(C10S)=Sof(H10S)=Sof(C9S)=Sof(H9S)=Sof(C8S)=Sof(C14S)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C13S)=Sof(H13S)=Sof(C12S)=Sof(H12S)=Sof(C11S)=Sof(H11S)=1-FVAR(1)
 Sof(C6S)=Sof(H6S)=Sof(C2S)=Sof(H2S)=Sof(C1S)=Sof(C5S)=Sof(H5S)=Sof(C4S)=
 Sof(H4S)=Sof(C3S)=Sof(H3S)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C19(H19), C22(H22)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C15(H15), C14(H14), C13(H13), C12(H12), C30(H30), C29(H29),
 C28(H28), C27(H27), C17(H17), C18(H18), C6S(H6S), C2S(H2S), C5S(H5S), C4S(H4S),
  C3S(H3S), C10S(H10S), C9S(H9S), C13S(H13S), C12S(H12S), C11S(H11S)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C7S(H7SA,H7SB,H7SC), C14S(H14A,H14B,H14C)
;
_shelx_res_checksum              20081
_olex2_submission_special_instructions 'No special instructions were received'