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_7046618
_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_absolute_configuration ad
_chemical_formula_moiety         'C54 H74 Cl2 O4 Ti, 2(C2 H3 N)'
_chemical_formula_sum            'C58 H80 Cl2 N2 O4 Ti'
_chemical_formula_weight         988.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'A 2y'
_space_group_name_H-M_alt        'A 1 2 1'
_symmetry_space_group_name_Hall  'A 2y'
_symmetry_space_group_name_H-M   'A 1 2 1'
_atom_sites_solution_hydrogens   geom
_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                 101.229(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2312(16)
_cell_length_b                   12.1620(8)
_cell_length_c                   27.103(2)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      22.4990
_cell_measurement_theta_min      3.4299
_cell_volume                     5571.1(8)
_computing_cell_refinement
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_collection
;
 CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_reduction
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'SHELXL-2016/6 (Sheldrick, 2016) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1442
_diffrn_reflns_av_unetI/netI     0.2212
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30661
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.499
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_min         3.506
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
 Empirical absorption correction using spherical harmonics,
  implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
; 
 Flack x determined using 1036 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3472
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01992d1.cif
_cod_data_source_block           1_2MeCN
_cod_depositor_comments
'Adding full bibliography for 7046618--7046620.cif.'
_cod_database_code               7046618
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              63149
_shelx_fab_checksum              58115