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_7703119
_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         'C33 H41 Br Cl2 O3 Ti, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C35 H45 Br Cl2 O3.5 Ti'
_chemical_formula_weight         720.42
_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                78.765(2)
_cell_angle_beta                 80.424(2)
_cell_angle_gamma                89.325(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1016(2)
_cell_length_b                   13.3903(3)
_cell_length_c                   24.3259(5)
_cell_measurement_reflns_used    26843
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.9600
_cell_measurement_theta_min      2.4410
_cell_volume                     3496.62(13)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.997
_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    2.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00  90.00  360
  3  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00 180.00  360
  4  \w   -110.00  70.00   0.50    2.00    --  -20.00  45.00 270.00  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      -0.0005935000
_diffrn_orient_matrix_UB_12      0.0336240000
_diffrn_orient_matrix_UB_13      -0.0263726000
_diffrn_orient_matrix_UB_21      -0.0132950000
_diffrn_orient_matrix_UB_22      0.0410544000
_diffrn_orient_matrix_UB_23      0.0144232000
_diffrn_orient_matrix_UB_31      0.0634281000
_diffrn_orient_matrix_UB_32      0.0100971000
_diffrn_orient_matrix_UB_33      -0.0023775000
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57804
_diffrn_reflns_point_group_measured_fraction_full 0.997
_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         2.551
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93419
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The unit cell contains 2 THF molecules which have been treated
as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         16124
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0378P)^2^+2.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11177
_reflns_number_total             16124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03969d2.cif
_cod_data_source_block           pmeoobrticl2_sq
_cod_original_formula_sum        'C35 H45 Br Cl2 O3.50 Ti'
_cod_database_code               7703119
_platon_squeeze_void_probe_radius 1.20