Synthesis, crystal structure, and cytotoxicity studies of titanacalix[4 and 8]arene complexes.
Miller-Shakesby, David M; Nigam, Shubhanchi; Hughes, David L.; Lopez-Estelles, Enrique; Elsegood, Mark R. J.; Cawthorne, Christopher J.; Archibald, Stephen J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8992–8999; doi:10.1039/c8dt01992d

data_7046620
_publ_section_title
;
 Synthesis, crystal structure, and cytotoxicity studies of titanacalix[4
 and 8]arene complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8992
_journal_page_last               8999
_journal_paper_doi               10.1039/c8dt01992d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C98 H127 Cl O9 Ti2, 7.25(C2 H3 N)'
_chemical_formula_sum            'C112.5 H148.75 Cl N7.25 O9 Ti2'
_chemical_formula_weight         1877.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.480(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.816(2)
_cell_length_b                   13.2305(9)
_cell_length_c                   32.648(3)
_cell_measurement_reflns_used    55457
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     11215.2(15)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.823
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.1220
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35666
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'Bruker-Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             4030
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         12068
_refine_ls_number_restraints     725
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1868
_refine_ls_R_factor_gt           0.1222
_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^)+(0.0391P)^2^+114.3493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7470
_reflns_number_total             12068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01992d1.cif
_cod_data_source_block           2_7_25MeCN
_cod_depositor_comments
'Adding full bibliography for 7046618--7046620.cif.'
_cod_original_formula_sum        'C112.50 H148.75 Cl N7.25 O9 Ti2'
_cod_database_code               7046620
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              47100
_shelx_fab_checksum              10928