Hydrazido complexes prepared by methylation of an anionic end-on bridging dinitrogen dititanium complex.
Ishida, Yutaka; Nakanishi, Yusuke; Hiratsuka, Takuma; Kawaguchi, Hiroyuki; Chemical communications (Cambridge, England) 60 (2024) 7459–7462; doi:10.1039/d4cc02080d

data_7133262
_publ_section_title
;
 Hydrazido complexes prepared by methylation of an anionic end-on bridging
 dinitrogen dititanium complex.
;
_journal_issue                   58
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7459
_journal_page_last               7462
_journal_paper_doi               10.1039/d4cc02080d
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C96 H146 K2 N2 O10 Ti2, 2(C6 H6)'
_chemical_formula_sum            'C108 H158 K2 N2 O10 Ti2'
_chemical_formula_weight         1818.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-24 deposited with the CCDC.	2024-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.92000(10)
_cell_length_b                   25.4342(2)
_cell_length_c                   30.2821(2)
_cell_measurement_reflns_used    25450
_cell_measurement_temperature    123
_cell_measurement_theta_max      76.1720
_cell_measurement_theta_min      2.9670
_cell_volume                     10439.94(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.100a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_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     35.00  76.00   0.50    0.18    --   39.20-141.00 135.00   82
  2  \w     57.00  83.00   0.50    0.72    --  113.00-141.00 135.00   52
  3  \w     87.00 120.00   0.50    0.72    --  113.00-141.00 135.00   66
  4  \w     75.00 100.00   0.50    0.72    --  113.00-111.00 150.00   50
  5  \w     39.00  64.00   0.50    0.72    --  113.00-111.00 150.00   50
  6  \w     83.00 108.00   0.50    0.72    --  113.00-111.00   0.00   50
  7  \w     69.00  95.00   0.50    0.72    --  113.00-128.00 -52.00   52
  8  \w     38.00  64.00   0.50    0.72    --  113.00-111.00 -60.00   52
  9  \w     37.00  73.00   0.50    0.72    --  113.00-111.00-150.00   72
 10  \w     36.00  72.00   0.50    0.72    --  113.00 -94.00-180.00   72
 11  \w     61.00 108.00   0.50    0.72    --  113.00-111.00-120.00   94
 12  \w     76.00 105.00   0.50    0.72    --  113.00-111.00 -60.00   58
 13  \w     65.00 106.00   0.50    0.72    --  113.00 -94.00 -30.00   82
 14  \w     80.00 108.00   0.50    0.72    --  113.00-111.00  60.00   56
 15  \w     36.00  77.00   0.50    0.72    --  113.00 -94.00  60.00   82
 16  \w     38.00  77.00   0.50    0.72    --  113.00 -61.00 120.00   78
 17  \w     52.00  77.00   0.50    0.72    --  113.00 -61.00   0.00   50
 18  \w    -21.00   6.00   0.50    0.18    --   39.20 -19.00 -60.00   54
 19  \w     48.00  73.00   0.50    0.72    --  113.00 -61.00-180.00   50
 20  \w    127.00 176.00   0.50    0.72    --  113.00  30.00-150.00   98
 21  \w     97.00 122.00   0.50    0.72    --  113.00 141.00-166.00   50
 22  \w     57.00 137.00   0.50    0.72    --  113.00 178.00 -30.00  160
 23  \w     96.00 122.00   0.50    0.72    --  113.00 128.00  21.00   52
 24  \w     86.00 176.00   0.50    0.72    --  113.00  61.00   0.00  180
 25  \w     85.00 166.00   0.50    0.72    --  113.00  61.00 -60.00  162
 26  \w     15.00  42.00   0.50    0.18    --  -39.20  19.00 -90.00   54
 27  \w      9.00  43.00   0.50    0.18    --  -39.20  19.00-150.00   68
 28  \w    -65.00 -26.00   0.50    0.72    -- -102.00  61.00-150.00   78
 29  \w     -6.00  43.00   0.50    0.18    --  -39.20  19.00  90.00   98
 30  \w    -34.00  42.00   0.50    0.18    --  -39.20  37.00 150.00  152
 31  \w   -108.00 -68.00   0.50    0.72    -- -102.00 111.00 -60.00   80
 32  \w    -57.00 -15.00   0.50    0.18    --  -39.20 128.00  21.00   84
 33  \w   -108.00 -32.00   0.50    0.18    --  -39.20 141.00-166.00  152
 34  \w    -99.00 -74.00   0.50    0.72    -- -102.00 141.00-166.00   50
 35  \w   -171.00 -84.00   0.50    0.72    -- -102.00 -94.00 -90.00  174
 36  \w   -142.00 -95.00   0.50    0.72    -- -102.00-128.00 -52.00   94
 37  \w   -113.00 -88.00   0.50    0.18    --  -39.20-141.00 135.00   50
 38  \w   -142.00-117.00   0.50    0.72    -- -102.00-141.00 135.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0306315000
_diffrn_orient_matrix_UB_12      -0.0583118000
_diffrn_orient_matrix_UB_13      -0.0024745000
_diffrn_orient_matrix_UB_21      -0.1067577000
_diffrn_orient_matrix_UB_22      0.0161314000
_diffrn_orient_matrix_UB_23      -0.0001406000
_diffrn_orient_matrix_UB_31      -0.0240952000
_diffrn_orient_matrix_UB_32      0.0027565000
_diffrn_orient_matrix_UB_33      -0.0521868000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            42396
_diffrn_reflns_point_group_measured_fraction_full 0.681
_diffrn_reflns_point_group_measured_fraction_max 0.665
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.495
_diffrn_reflns_theta_min         2.997
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.073(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         14592
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0788P)^2^+4.1753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.357
_reflns_Friedel_fraction_full    0.364
_reflns_Friedel_fraction_max     0.350
_reflns_number_gt                14001
_reflns_number_total             14592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02080d2.cif
_cod_data_source_block           ti_o3c_n2_me2_k
_cod_depositor_comments
'Adding full bibliography for 7133261--7133262.cif.'
_cod_database_code               7133262
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.628
_shelx_res_checksum              71517
_shelx_hkl_checksum              85920
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.770