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

data_7713564
_publ_section_title
;
 N-Aryloxide-Amidinate Group 4 Metal Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01767B
_journal_year                    2023
_chemical_formula_moiety         '2(C24 H31 Cl Hf N2 O2)'
_chemical_formula_sum            'C48 H62 Cl2 Hf2 N4 O4'
_chemical_formula_weight         1186.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                100.1710(10)
_cell_angle_beta                 109.6060(10)
_cell_angle_gamma                103.6480(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2507(2)
_cell_length_b                   13.1833(2)
_cell_length_c                   16.8154(2)
_cell_measurement_reflns_used    39510
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.7170
_cell_measurement_theta_min      3.0100
_cell_volume                     2387.07(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_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    -21.00  88.00   0.50    0.50    --   -1.70  38.00-150.00  218
  2  \w    -32.00  84.00   0.50    0.50    --   -1.70  77.00   0.00  232
  3  \w     24.00  72.00   0.50    0.50    --   -1.70  77.00-120.00   96
  4  \w    -25.00  76.00   0.50    0.50    --   -1.70  57.00 -30.00  202
  5  \w    -32.00   2.00   0.50    0.50    --   -1.70  77.00-120.00   68
  6  \w    -25.00  79.00   0.50    0.50    --   -1.70  57.00 120.00  208
  7  \w    -32.00  80.00   0.50    0.50    --   -1.70  77.00  60.00  224
  8  \w     -6.00  26.00   0.50    0.50    --    1.90 -19.00 -60.00   64
  9  \w    -82.00 -23.00   0.50    0.50    --    1.90 -19.00 -60.00  118
;
_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      0.0120580000
_diffrn_orient_matrix_UB_12      0.0288024000
_diffrn_orient_matrix_UB_13      0.0434580000
_diffrn_orient_matrix_UB_21      -0.0587603000
_diffrn_orient_matrix_UB_22      0.0064013000
_diffrn_orient_matrix_UB_23      -0.0148046000
_diffrn_orient_matrix_UB_31      -0.0246083000
_diffrn_orient_matrix_UB_32      -0.0495422000
_diffrn_orient_matrix_UB_33      0.0081871000
_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  0.0742
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.590
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.43a (Rigaku Oxford Diffraction, 2019)
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    1.651
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.453
_refine_diff_density_min         -2.412
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9933
_reflns_number_total             10906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01767b2.cif
_cod_data_source_block           exp_10622
_cod_original_cell_volume        2387.07(6)
_cod_database_code               7713564
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Hf Cl C H O N'
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.915
_reflns_odcompleteness_completeness 99.88
_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:
 C00G(H00I,H00J), C00H(H00D,H00E), C00Z(H00R,H00S), C017(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00V(H00V), C012(H012), C015(H015), C016(H016), C019(H019),
 C01A(H01C), C01C(H01Z), C01E(H01G), C01F(H01H), C01I(H01), C01J(H01O)
2.c Idealised Me refined as rotating group:
 C00E(H00A,H00B,H00C), C00W(H00K,H00L,H00M), C00X(H00O,H00P,H00Q), C00Y(H00F,
 H00G,H00H), C013(H01V,H01W,H01X), C018(H01Y,H,HA), C01B(H01D,H01E,H01F),
 C01G(H01I,H01J,H01K), C01H(H01L,H01M,H01N), C01K(H01P,H01Q,H01R), C01L(H01S,
 H01T,H01U), C01M(H1,HB,HC), C01N(H2,HD,HE), C01O(H3,HF,HG)
;
_shelx_res_checksum              19507
_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 3.965
_oxdiff_exptl_absorpt_empirical_full_min 0.455