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_7133261
_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_formula_moiety         'C130 H190 K2 N2 O24 Ti2, 1[C6H6], 2[C4H8O]'
_chemical_formula_sum            'C144 H212 K2 N2 O26 Ti2'
_chemical_formula_weight         2561.14
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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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.
;
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_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   -110.00  70.00   0.50   32.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50   32.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50   32.00    --  -20.00  45.00 180.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220070000
_diffrn_orient_matrix_UB_12      0.0002084000
_diffrn_orient_matrix_UB_13      -0.0261658000
_diffrn_orient_matrix_UB_21      0.0440435000
_diffrn_orient_matrix_UB_22      0.0131890000
_diffrn_orient_matrix_UB_23      0.0158516000
_diffrn_orient_matrix_UB_31      0.0193269000
_diffrn_orient_matrix_UB_32      -0.0287860000
_diffrn_orient_matrix_UB_33      0.0002701000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1105
_diffrn_reflns_av_unetI/netI     0.1959
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            89349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         2.593
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88532
_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            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       plate
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1527
_refine_ls_number_reflns         32875
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.2061
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1024P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14658
_reflns_number_total             32875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02080d2.cif
_cod_data_source_block           o3ctinme_co2
_cod_depositor_comments
'Adding full bibliography for 7133261--7133262.cif.'
_cod_database_code               7133261
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.939
_shelx_res_checksum              7532
_shelx_hkl_checksum              53353
_shelx_fab_checksum              29945
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.670