First-row early transition metal complexes with a highly sterically demanding triisopropylphenyl amino triphenolate ligand: synthesis and applications
Bae, Dae Young; Park, Gyeong Su; Ko, Nakeun; Son, Kyung-sun; Lee, Eunsung; Dalton Transactions  (2019) –; doi:10.1039/C9DT00456D

data_7049156
_publ_section_title
;
 First-row early transition metal complexes with a highly sterically
 demanding triisopropylphenyl amino triphenolate ligand: synthesis and
 applications
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00456D
_journal_year                    2019
_chemical_formula_moiety         'C69 H91 N1 O4 Ti1, 3.5(C6 H6)'
_chemical_formula_sum            'C90 H112 N O4 Ti'
_chemical_formula_weight         1319.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-12
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.02.04 svn.r3569 for OlexSys, GUI svn.r5585)
;
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   23.4039(2)
_cell_length_b                   23.4039(2)
_cell_length_c                   24.9083(5)
_cell_measurement_reflns_used    38020
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.427
_cell_measurement_theta_min      1.295
_cell_volume                     11815.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38020
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.427
_diffrn_reflns_theta_min         1.295
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             4278
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.146
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         12774
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1422P)^2^+10.1453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7853
_reflns_number_total             12774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00456d2.cif
_cod_data_source_block           r-3
_cod_database_code               7049156
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 C1-O2
 1.4248 with sigma of 0.02
 O2-C1A
 2.3732 with sigma of 0.04
 O2-C2
 2.4353 with sigma of 0.04
 C2-C1A
 2.5114 with sigma of 0.04
 C1-C2 \\sim C1-C1A
 with sigma of 0.02
 C2-C1 \\sim C1A-C1
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1A) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O2) = Uanis(O2) = Uanis(O2)
4. Rigid body (RIGU) restrains
 O2, C1, C2, C1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O2(0.33333) C1(0.33333) H1(0.33333) C2(0.33333) H2A(0.33333)
 H2B(0.33333) H2C(0.33333) C1A(0.33333) H1AA(0.33333) H1AB(0.33333)
 H1AC(0.33333)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C9(H9), C1(H1)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C22(H22), C23(H23), C4(H4), C28(H28), C30(H30), C31(H31),
 C27(H27), C29(H29), C26(H26), C8(H8)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C2(H2A,H2B,H2C), C1A(H1AA,
 H1AB,H1AC)
;
_shelx_res_checksum              25948
_shelx_hkl_checksum              8396
_olex2_submission_special_instructions 'No special instructions were received'