Synthesis of asymmetrical diaminobis(alkoxo)-bisphenol compounds and their C<sub>1</sub>-symmetrical mono-ligated titanium(iv) complexes as highly stable highly active antitumor compounds.
Nahari, Gilad; Tshuva, Edit Y.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6423–6426; doi:10.1039/d1dt00219h

data_7707317
_publ_section_title
;
 Synthesis of asymmetrical diaminobis(alkoxo)-bisphenol compounds and
 their C<sub>1</sub>-symmetrical mono-ligated titanium(iv) complexes as
 highly stable highly active antitumor compounds.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6423
_journal_page_last               6426
_journal_paper_doi               10.1039/d1dt00219h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C20 H21 Br2 N3 O6 Ti, C H2 Cl2'
_chemical_formula_sum            'C21 H23 Br2 Cl2 N3 O6 Ti'
_chemical_formula_weight         692.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-24
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.976(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0658(2)
_cell_length_b                   24.2061(4)
_cell_length_c                   10.8597(2)
_cell_measurement_reflns_used    18867
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.6140
_cell_measurement_theta_min      2.1420
_cell_volume                     2516.84(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.885
_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     -4.00  82.00   0.50   70.00    --    9.19  37.00   0.00  172
  2  \w     -1.00  46.00   0.50   70.00    --    9.19-107.00-141.00   94
  3  \w    -21.00  44.00   0.50   70.00    --    9.19 -99.00   0.00  130
  4  \w     -1.00  25.00   0.50   70.00    --  -10.44 -99.00  30.00   52
  5  \w    -20.00   6.00   0.50   70.00    --  -10.44 -57.00  90.00   52
  6  \w    -22.00  22.00   0.50   70.00    --  -10.44 -99.00  60.00   88
  7  \w    -24.00   7.00   0.50   70.00    --  -10.44 -99.00-120.00   62
  8  \w    -23.00  35.00   0.50   70.00    --    9.19 -99.00-180.00  116
  9  \w    -17.00  14.00   0.50   70.00    --  -10.44 -99.00-150.00   62
 10  \w    -49.00   5.00   0.50   70.00    --    9.19 -19.00-180.00  108
 11  \w    -40.00 -14.00   0.50   70.00    --  -10.44 107.00 -43.00   52
 12  \w    -83.00 -48.00   0.50   70.00    --  -10.44 -57.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0739924000
_diffrn_orient_matrix_UB_12      0.0012328000
_diffrn_orient_matrix_UB_13      0.0226305000
_diffrn_orient_matrix_UB_21      -0.0025866000
_diffrn_orient_matrix_UB_22      0.0284226000
_diffrn_orient_matrix_UB_23      -0.0164967000
_diffrn_orient_matrix_UB_31      -0.0023515000
_diffrn_orient_matrix_UB_32      0.0070244000
_diffrn_orient_matrix_UB_33      0.0627006000
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46034
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.211
_diffrn_reflns_theta_min         2.127
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.771
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0296P)^2^+4.0692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6539
_reflns_number_total             7875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00219h2.cif
_cod_data_source_block           L34Ti
_cod_depositor_comments          'Adding full bibliography for 7707317.cif.'
_cod_database_code               7707317
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H21 N3 O6 Br2 Ti'
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.418
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl2S(0.8) Cl3S(0.2) C1SA(0.8) H1SA(0.8) H1SB(0.8) C1SB(0.2)
 H1SC(0.2) H1SD(0.2)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C1SA(H1SA,H1SB), C1SB(H1SC,
 H1SD)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C18(H18), C20(H20)
;
_shelx_res_checksum              36876
_shelx_hkl_checksum              37828
_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.790