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

data_7713563
_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 N2 O2 Zr)'
_chemical_formula_sum            'C48 H62 Cl2 N4 O4 Zr2'
_chemical_formula_weight         1012.35
_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             2022-11-24
_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                101.875(2)
_cell_angle_beta                 109.119(2)
_cell_angle_gamma                104.700(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3616(3)
_cell_length_b                   13.1320(3)
_cell_length_c                   16.7306(4)
_cell_measurement_reflns_used    27867
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.0990
_cell_measurement_theta_min      2.6700
_cell_volume                     2354.85(11)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -79.00 -44.00   0.50    0.50    --   -8.20 -38.00-120.00   70
  2  \w    -30.00  98.00   0.50    0.50    --    8.20  77.00  60.00  256
  3  \w    -49.00 -11.00   0.50    0.50    --    8.20 -38.00  60.00   76
  4  \w    -12.00  14.00   0.50    0.50    --    8.20  57.00 -60.00   52
  5  \w     53.00  79.00   0.50    0.50    --    8.20  57.00 -60.00   52
  6  \w    -81.00  37.00   0.50    0.50    --    8.20 -57.00   0.00  236
  7  \w    -26.00  11.00   0.50    0.50    --    8.20 -77.00-120.00   74
  8  \w    -80.00  31.00   0.50    0.50    --    8.20 -77.00 -30.00  222
  9  \w    -18.00  88.00   0.50    0.50    --    8.20  57.00-150.00  212
;
_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      0.0359272000
_diffrn_orient_matrix_UB_12      -0.0340140000
_diffrn_orient_matrix_UB_13      -0.0023228000
_diffrn_orient_matrix_UB_21      -0.0537898000
_diffrn_orient_matrix_UB_22      -0.0476761000
_diffrn_orient_matrix_UB_23      -0.0219463000
_diffrn_orient_matrix_UB_31      -0.0031498000
_diffrn_orient_matrix_UB_32      0.0058656000
_diffrn_orient_matrix_UB_33      -0.0418310000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_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            41430
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.560
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15832
_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    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.0691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9822
_reflns_number_total             10762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01767b2.cif
_cod_data_source_block           exp_9747
_cod_original_cell_volume        2354.84(10)
_cod_database_code               7713563
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zr Cl'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.988
_reflns_odcompleteness_completeness 99.80
_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:
 C15(H15A,H15B), C11(H11A,H11B), C39(H39A,H39B), C43(H43A,H43B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C22(H22), C7(H7), C6(H6), C36(H36), C21(H21), C50(H50), C34(H34),
 C20(H20), C35(H35), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C16(H16A,H16B,H16C), C44(H44A,H44B,H44C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C25(H25A,H25B,H25C), C55(H55A,H55B,H55C),
 C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              40548
_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 2.363
_oxdiff_exptl_absorpt_empirical_full_min 0.543