Single-crystal-to-single-crystal desolvation in a Ti32 nanoring cluster
Wang, Xiangxiang; Gui, Daxiang; Zhai, Fuwan; Li, Hui; Wang, Xia; Wang, Yanlong; Chen, Lanhua; Zheng, Tao; Chai, Zhifang; Wang, Shuao; CrystEngComm 20 (2018) 7062–; doi:10.1039/C8CE00717A

data_7231665
_publ_section_title
;
 Single-crystal-to-single-crystal desolvation in a Ti32 nanoring cluster
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              7062
_journal_paper_doi               10.1039/C8CE00717A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C319 H608 N16 O197 Ti32'
_chemical_formula_weight         9352.07
_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   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-09-13 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                81.041(12)
_cell_angle_beta                 79.236(6)
_cell_angle_gamma                66.339(11)
_cell_formula_units_Z            2
_cell_length_a                   21.009(10)
_cell_length_b                   23.513(15)
_cell_length_c                   44.73(2)
_cell_measurement_reflns_used    8827
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.20
_cell_volume                     19802(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_publication_material  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1301
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            426865
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        21.000
_diffrn_reflns_theta_max         21.000
_diffrn_reflns_theta_min         0.931
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_description       block
_exptl_crystal_F_000             6796
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00363(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3623
_refine_ls_number_reflns         41953
_refine_ls_number_restraints     6983
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1594P)^2^+127.7323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29793
_reflns_number_total             42557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00717a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7231664--7231665.cif.'
_cod_database_code               7231665
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              82895
_shelx_fab_checksum              65938