A butterfly-like lead-doped titanium-oxide compound with high performance in photocatalytic cycloaddition of CO<sub>2</sub> to epoxide.
Said, Amir; Zhang, Guanyun; Liu, Caiyun; Wang, Dexin; Niu, Huihui; Liu, Yanshu; Chen, Guanjie; Tung, Chen-Ho; Wang, Yifeng; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2392–2403; doi:10.1039/d2dt03990g

data_7712175
_publ_section_title
;
 A butterfly-like lead-doped titanium-oxide compound with high performance
 in photocatalytic cycloaddition of CO<sub>2</sub> to epoxide.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2392
_journal_page_last               2403
_journal_paper_doi               10.1039/d2dt03990g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C72 H68 N8 O40 Pb2 Ti10, C3 H7 N O'
_chemical_formula_sum            'C75 H75 N9 O41 Pb2 Ti10'
_chemical_formula_weight         2651.82
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-22 deposited with the CCDC.	2023-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.317(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.7509(10)
_cell_length_b                   19.9772(6)
_cell_length_c                   31.9410(8)
_cell_measurement_temperature    172.9(10)
_cell_volume                     26925.4(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      172.9(10)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74476
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.767
_diffrn_reflns_theta_min         2.869
_exptl_absorpt_coefficient_mu    10.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAliPro1.171.40.19a (Rigaku Oxford Diffraction)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       block
_exptl_crystal_F_000             10400
_exptl_crystal_preparation       'Solvothermal method'
_exptl_crystal_recrystallization_method 'Solvothermal method'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.309
_refine_diff_density_min         -1.973
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1295
_refine_ls_number_reflns         26051
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.1032
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1585P)^2^+379.1690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2827
_refine_ls_wR_factor_ref         0.2987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20600
_reflns_number_total             26051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03990g2.cif
_cod_data_source_block           c2c
_cod_depositor_comments          'Adding full bibliography for 7712175.cif.'
_cod_database_code               7712175
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.008
_shelx_estimated_absorpt_t_min   0.007
_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. Restrained distances
 C62-C61
 1.5 with sigma of 0.02
 C56-C55
 1.45 with sigma of 0.02
 O41-C73
 1.28 with sigma of 0.02
 N9-C72 = N9-C71 = N9-C73
 1.45 with sigma of 0.02
 O42-C74
 1.28 with sigma of 0.02
 N10-C74 = N10-C75 = N10-C76
 1.45 with sigma of 0.02
 C47-C48 = N8-C47 = C43-C47
 1.41 with sigma of 0.02
 O4-C61
 1.28 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23 \\sim O24 \\sim C69 \\sim C70: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N7 \\sim N8 \\sim C40 \\sim C43 \\sim C46 \\sim C47 \\sim C48: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O25 \\sim O26 \\sim C65 \\sim C66: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O42 \\sim N10 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O41 \\sim N9 \\sim C71 \\sim C72 \\sim C73: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: O41(0.5) N9(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) C72(0.5)
 H72A(0.5) H72B(0.5) H72C(0.5) C73(0.5) H73(0.5) O42(0.5) N10(0.5) C74(0.5)
 H74(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) C76(0.5) H76A(0.5) H76B(0.5)
 H76C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C73(H73), C74(H74)
5.b Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,
 H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C78(H78A,H78B,H78C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C75(H75A,H75B,
 H75C), C76(H76A,H76B,H76C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1160 electrons were 
found in a volume of 10074\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.085[C3H7NO] per Unit Cell 
which account for 1160 electrons 
per unit cell.
;
_shelx_res_checksum              73036
_shelx_hkl_checksum              60312
_shelx_fab_checksum              81957
_olex2_submission_special_instructions 'No special instructions were received'