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_7046619
_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
'C94.62 H116.35 Cl2.69 N2 O11.96 Si1.31 Ti4, 10(C2 H3 N)'
_chemical_formula_sum
'C114.62 H146.35 Cl2.69 N12 O11.96 Si1.31 Ti4'
_chemical_formula_weight         2207.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-06-08 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.2143(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.7283(3)
_cell_length_b                   14.26944(14)
_cell_length_c                   28.7967(3)
_cell_measurement_reflns_used    59808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5610
_cell_measurement_theta_min      1.5920
_cell_volume                     12154.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT, (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
; 
Rigaku FRE+ equipped with HF Varimax confocal mirrors 
and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            97082
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Cut Needle'
_exptl_crystal_F_000             4663
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         13919
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0478P)^2^+36.0626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13137
_reflns_number_total             13919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01992d1.cif
_cod_data_source_block           cr543
_cod_depositor_comments
'Adding full bibliography for 7046618--7046620.cif.'
_cod_database_code               7046619
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              52978