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_7049157
_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         'C66 H87 N O3, C4 H8 O'
_chemical_formula_sum            'C70 H95 N O4'
_chemical_formula_weight         1014.46
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-29 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.81(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.089(4)
_cell_length_b                   9.862(2)
_cell_length_c                   27.858(6)
_cell_measurement_reflns_used    37868
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.465
_cell_volume                     6055(2)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70000
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37868
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.465
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0621
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6568
_reflns_number_total             10276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00456d2.cif
_cod_data_source_block           p21c
_cod_database_code               7049157
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.995
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C54(H54), C29(H29), C57(H57), C51(H51), C32(H32),
 C35(H35), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C22(H22A,H22B), C44(H44A,H44B), C70(H70A,H70B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B)
2.c Aromatic/amide H refined with riding coordinates:
 C63(H63), C61(H61), C62(H62), C19(H19), C46(H46), C50(H50), C18(H18),
 C24(H24), C17(H17), C6(H6), C28(H28), C2(H2A), C41(H41), C43(H43), C42(H42)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C56(H56A,H56B,H56C), C14(H14A,H14B,H14C), C55(H55A,H55B,
 H55C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C58(H58A,H58B,H58C), C36(H36A,
 H36B,H36C), C30(H30A,H30B,H30C), C59(H59A,H59B,H59C), C8(H8A,H8B,H8C),
 C52(H52A,H52B,H52C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C53(H53A,H53B,H53C),
  C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O2(H2)
;
_shelx_res_checksum              95888
_shelx_hkl_checksum              98113
_olex2_submission_special_instructions 'No special instructions were received'