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_7049155
_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         'C70 H92 N O4 V'
_chemical_formula_sum            'C70 H92 N O4 V'
_chemical_formula_weight         1062.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.33(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.206(7)
_cell_length_b                   14.294(3)
_cell_length_c                   24.650(5)
_cell_measurement_reflns_used    10736
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.527
_cell_volume                     13053(5)
_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 0.963
_diffrn_measured_fraction_theta_max 0.963
_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     0.7000
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19755
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.527
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light navy'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    navy
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10736
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0862
_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^)+(0.1599P)^2^+30.3613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2498
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9784
_reflns_number_total             10736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00456d2.cif
_cod_data_source_block           c2c_1
_cod_database_code               7049155
_shelx_shelxl_version_number     2016/4
_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. Uiso/Uaniso restraints and constraints
Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.2
3. Others
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C57(H57), C32(H32), C10(H10), C35(H35), C54(H54), C13(H13), C51(H51),
 C29(H29), C7(H7A), C7(H7B)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C66(H66A,H66B), C44(H44A,H44B), C70(H70A,H70B), C69(H69A,
 H69B), C68(H68A,H68B), C67(H67A,H67B)
4.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C63(H63), C40(H40), C61(H61), C41(H41), C62(H62), C17(H17),
 C19(H19), C50(H50), C46(H46), C18(H18), C24(H24), C28(H28), C6(H6), C2(H2)
4.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C12(H12A,H12B,H12C), C37(H37A,H37B,
 H37C), C11(H11A,H11B,H11C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C), C34(H34A,
 H34B,H34C), C33(H33A,H33B,H33C), C55(H55A,H55B,H55C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C),
  C9(H9A,H9B,H9C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C9A(H9AA,H9AB,H9AC)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 172.0 electrons were 
found in a volume of 1164.0 A^3 in 3 voids. 
This is consistent with the presence of 
4 [n-pentane] per formula unit 
which account for 168.0 electrons.
;
_shelx_res_checksum              40887
_shelx_hkl_checksum              55452
_shelx_fab_checksum              87402
_olex2_submission_special_instructions 'No special instructions were received'