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_7049154
_publ_section_title
;
 First-row early transition metal complexes with a highly sterically
 demanding triisopropylphenyl amino triphenolate ligand: synthesis and
 applications
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00456D
_journal_year                    2019
_chemical_formula_moiety         'C70 H92 Cr N O4'
_chemical_formula_sum            'C72.5 H98 Cr N O4'
_chemical_formula_weight         1099.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                108.161(3)
_cell_angle_beta                 91.379(3)
_cell_angle_gamma                110.604(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1640(11)
_cell_length_b                   14.4132(11)
_cell_length_c                   18.4865(14)
_cell_measurement_reflns_used    108134
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      1.173
_cell_volume                     3318.4(5)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_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       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            108134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.173
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         11295
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0655P)^2^+3.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10052
_reflns_number_total             11295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00456d2.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        3318.4(4)
_cod_original_formula_sum        'C72.50 H98 Cr N O4'
_cod_database_code               7049154
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_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. Uiso/Uaniso restraints and constraints
Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.05
3. Others
 Sof(H29A)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(H29)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Fixed Sof: H7A(0.5) H7B(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5) C9B(0.5)
 H9BA(0.5) H9BB(0.5) H9BC(0.5)
4.a Ternary CH refined with riding coordinates:
 C54(H54), C13(H13), C32(H32), C35(H35), C57(H57), C10(H10), C51(H51),
 C29(H29), C29(H29A), C7(H7A), C7(H7B)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C22(H22A,H22B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,
 H69B), C70(H70A,H70B), C68(H68A,H68B)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C43(H43), C63(H63), C61(H61), C18(H18), C41(H41), C62(H62),
 C17(H17), C42(H42), C28(H28), C50(H50), C46(H46), C24(H24), C2(H2), C6(H6)
4.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,
 H59C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C58(H58A,H58B,H58C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C8(H8A,H8B,H8C), C30(H30A,H30B,H30C),
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C52(H52A,H52B,H52C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C31A(H31A,H31B,H31C), C31(H31D,H31E,H31F),
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 75.8 electrons were 
found in a volume of 426.5 A^3 in one void. 
This is consistent with the presence of 
1.8 [n-pentane] per formula unit 
which account for 75.6 electrons.
;
_shelx_res_checksum              19481
_shelx_hkl_checksum              85513
_shelx_fab_checksum              74225
_olex2_submission_special_instructions 'No special instructions were received'