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_7249227
_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         'C28 H42 N6 O4 Ti'
_chemical_formula_sum            'C28 H42 N6 O4 Ti'
_chemical_formula_weight         574.57
_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             2022-02-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7949(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2014(7)
_cell_length_b                   10.7004(3)
_cell_length_c                   24.3975(7)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.60
_cell_volume                     6026.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0771
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            157194
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.538
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_recrystallization_method
'evaporation from saturated pentane solution'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         17589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+3.7815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15053
_reflns_number_total             17589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05146g2.cif
_cod_data_source_block           zn001_0m
_cod_database_code               7249227
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.968
_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. Others
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28B)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C29B)=Sof(H29B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C26A(H26A), C29A(H29A), C23A(H23A), C23B(H23B), C29B(H29B), C26B(H26B)
3.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C3A(H3AA,H3AB), C13A(H13A,H13B), C14A(H14A,H14B), C2B(H2BB,
 H2BA), C3B(H3BA,H3BB), C13B(H13C,H13D), C14B(H14C,H14D)
3.c Aromatic/amide H refined with riding coordinates:
 C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C19A(H19A), C20A(H20A),
 C21A(H21A), C22A(H22A), C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C19B(H19B),
  C20B(H20B), C21B(H21B), C22B(H22B)
3.d Idealised Me refined as rotating group:
 C4A(H4AA,H4AC,H4AB), C5A(H5AA,H5AC,H5AB), C15A(H15B,H15C,H15A), C16A(H16A,
 H16B,H16C), C27A(H27A,H27B,H27C), C28A(H28C,H28A,H28B), C30A(H30A,H30B,H30C),
 C31A(H31A,H31B,H31C), C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C4B(H4BB,
 H4BC,H4BA), C5B(H5BA,H5BB,H5BC), C15B(H15E,H15F,H15D), C16B(H16D,H16E,H16F),
 C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C30B(H30D,H30E,H30F), C31B(H31D,
 H31E,H31F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F)
;
_shelx_res_checksum              8388
_olex2_submission_special_instructions 'No special instructions were received'