Synthesis and structures of titanium complexes bearing tetradentate tripodal [O<sub>2</sub>XC] ligands (X = C, P).
Nakanishi, Yusuke; Ishida, Yutaka; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 49 (2020) 27–30; doi:10.1039/c9dt03969d

data_7703121
_publ_section_title
;
 Synthesis and structures of titanium complexes bearing tetradentate
 tripodal [O<sub>2</sub>XC] ligands (X = C, P).
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              27
_journal_page_last               30
_journal_paper_doi               10.1039/c9dt03969d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C52 H59 Cl N O2 P Ti, 1(C7 H8)'
_chemical_formula_sum            'C59 H67 Cl N O2 P Ti'
_chemical_formula_weight         936.45
_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
_audit_creation_date             2019-10-01
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-07 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                79.141(1)
_cell_angle_beta                 80.483(1)
_cell_angle_gamma                84.749(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9944(2)
_cell_length_b                   13.2152(2)
_cell_length_c                   17.0702(3)
_cell_measurement_reflns_used    20127
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.2050
_cell_measurement_theta_min      2.2450
_cell_volume                     2615.65(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_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   -110.00  70.00   0.50    8.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    8.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    8.00    --  -20.00  45.00 180.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101110000
_diffrn_orient_matrix_UB_12      0.0076187000
_diffrn_orient_matrix_UB_13      -0.0427687000
_diffrn_orient_matrix_UB_21      -0.0126812000
_diffrn_orient_matrix_UB_22      0.0537831000
_diffrn_orient_matrix_UB_23      -0.0016782000
_diffrn_orient_matrix_UB_31      0.0578476000
_diffrn_orient_matrix_UB_32      0.0069139000
_diffrn_orient_matrix_UB_33      0.0003755000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32698
_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         2.674
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         12066
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0532P)^2^+0.9368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9547
_reflns_number_total             12066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03969d2.cif
_cod_data_source_block           oocpticl
_cod_database_code               7703121