N-Aryloxide-Amidinate Group 4 Metal Complexes
Xu, Hanhua; Lv, Ze-Jie; Wei, Junnian; Xi, Zhenfeng; Dalton Transactions  (2023) –; doi:10.1039/D3DT01767B

data_7713562
_publ_section_title
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 N-Aryloxide-Amidinate Group 4 Metal Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01767B
_journal_year                    2023
_chemical_formula_moiety         'C60 H94 Li6 N8 O4'
_chemical_formula_sum            'C60 H94 Li6 N8 O4'
_chemical_formula_weight         1033.07
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-29 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.260(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2159(6)
_cell_length_b                   14.3624(4)
_cell_length_c                   17.5594(4)
_cell_measurement_reflns_used    20582
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.3850
_cell_measurement_theta_min      2.0940
_cell_volume                     6357.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00 -52.00   0.50   15.94    --  -12.90 -19.00 120.00  100
  2  \w    -45.00  76.00   0.50   15.94    --  -12.90 -19.00 120.00  242
  3  \w    -78.00  34.00   0.50   15.94    --  -12.90 -37.00  60.00  224
  4  \w    -21.00   6.00   0.50   15.94    --   12.90  77.00-120.00   54
  5  \w    -11.00  75.00   0.50   15.94    --   12.90  57.00 -60.00  172
  6  \w     -5.00  20.00   0.50   15.94    --   12.90 -77.00  90.00   50
  7  \w    -27.00  37.00   0.50   15.94    --   12.90  82.00  60.00  128
  8  \w     -6.00  98.00   0.50   15.94    --   12.90  57.00  30.00  208
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0019313000
_diffrn_orient_matrix_UB_12      0.0439223000
_diffrn_orient_matrix_UB_13      -0.0183241000
_diffrn_orient_matrix_UB_21      0.0063083000
_diffrn_orient_matrix_UB_22      -0.0211336000
_diffrn_orient_matrix_UB_23      -0.0351625000
_diffrn_orient_matrix_UB_31      -0.0273546000
_diffrn_orient_matrix_UB_32      -0.0079802000
_diffrn_orient_matrix_UB_33      -0.0077379000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.079
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0628P)^2^+4.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6182
_reflns_number_total             7291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01767b2.cif
_cod_data_source_block           exp_8146
_cod_database_code               7713562
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Li'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.987
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C32(H32A,H32B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C2(H2), C18(H18), C17(H17), C3(H3)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,
 H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              91918
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.670
_oxdiff_exptl_absorpt_empirical_full_min 0.455