Titanium(iv)-based helicates incorporating the ortho-phenylenediamine ligand: a structural and a computational investigation
Baradel, Nathalie; Mobian, Pierre; Khalil, Georges; Henry, Marc; Dalton Trans.  (2017) –; doi:10.1039/C7DT00912G

data_7043221
_publ_section_title
;
 Titanium(iv)-based helicates incorporating the ortho-phenylenediamine
 ligand: a structural and a computational investigation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00912G
_journal_year                    2017
_chemical_formula_moiety         'C96 H68 N4 O8 Ti2, 2(C H2 Cl2)'
_chemical_formula_sum            'C98 H72 Cl4 N4 O8 Ti2'
_chemical_formula_weight         1841.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                112.394(2)
_cell_angle_beta                 98.802(2)
_cell_angle_gamma                103.4430(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2302(4)
_cell_length_b                   19.0950(6)
_cell_length_c                   20.3691(10)
_cell_measurement_reflns_used    67000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      2.5
_cell_volume                     4457.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67643
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         1.705
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         20467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1294P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2294
_refine_ls_wR_factor_ref         0.2584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11706
_reflns_number_total             20467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00912g2.cif
_cod_data_source_block           e2200n_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

2018-03-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C96 H68 N4 O8 Ti2, 4(C H2 Cl2)'
_cod_original_formula_sum        'C200 H152 Cl16 N8 O16 Ti4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3682.09
_cod_database_code               7043221
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2014/6
_shelx_res_checksum              57744
_shelx_fab_checksum              31999