Titanium-Based Nanoscale Metal-Organic Framework for Type I Photodynamic Therapy.
Lan, Guangxu; Ni, Kaiyuan; Veroneau, Samuel S.; Feng, Xuanyu; Nash, Geoffrey T.; Luo, Taokun; Xu, Ziwan; Lin, Wenbin; Journal of the American Chemical Society 141 (2019) 4204–4208; doi:10.1021/jacs.8b13804

data_4127478
_publ_section_title
;
 Titanium-Based Nanoscale Metal-Organic Framework for Type I Photodynamic
 Therapy.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4204
_journal_page_last               4208
_journal_paper_doi               10.1021/jacs.8b13804
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C50 H27 N4 O13 Ti3.5'
_chemical_formula_sum            'C50 H27 N4 O13 Ti3.5'
_chemical_formula_weight         1059.40
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.685(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.496(3)
_cell_length_b                   16.181(3)
_cell_length_c                   34.167(5)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.88
_cell_measurement_theta_min      2.19
_cell_volume                     9110(3)
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 30
_diffrn_detector_type            'CMOS pixel array detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Si(111) & Si(311)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            112970
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        11.944
_diffrn_reflns_theta_max         11.944
_diffrn_reflns_theta_min         0.975
_diffrn_source                   synchrotron
_diffrn_source_type
'Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7436
_exptl_absorpt_correction_T_min  0.5787
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.772
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         9554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.1439
_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^)+(0.1600P)^2^+62.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3692
_refine_ls_wR_factor_ref         0.3767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7987
_reflns_number_total             9554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13804_si_001.cif
_cod_data_source_block           1a
_cod_original_cell_volume        9110(2)
_cod_original_formula_sum        'C50 H27 N4 O13 Ti3.50'
_cod_database_code               4127478
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.998
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C18(H18), C44(H44), C8(H8), C19(H19), C13(H13), C9(H9), C41(H41),
 C34(H34), C40(H40), C38(H38), C26(H26), C25(H25), C23(H23), C22(H22), C14(H14),
  C37(H37), C35(H35), C31(H31), C29(H29), C32(H32), C3(H3), C28(H28), C4(H4)
2.b Fitted hexagon refined as free rotating group:
 C26(C25,C24,C23,C22,C21)
2.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C)
;
_shelx_res_checksum              6738
_shelx_hkl_checksum              11492
_shelx_fab_checksum              70473
_olex2_submission_special_instructions 'No special instructions were received'