Stepwise Assembly and Reversible Structure Transformation of Ligated Titanium Coated Bismuth-Oxo Cores: Shell Morphology Engineering for Enhanced Chemical Fixation of CO2
Zhang, Lei; Ding, Qing-Rong; Yu, Yinghua; Cao, Changsheng; Zhang, Jian; Chemical Science  (2022) –; doi:10.1039/D1SC06847D

data_1566242
_publ_section_title
;
 Stepwise Assembly and Reversible Structure Transformation of Ligated
 Titanium Coated Bismuth-Oxo Cores: Shell Morphology Engineering for
 Enhanced Chemical Fixation of CO2
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC06847D
_journal_year                    2022
_chemical_formula_moiety         'C312 H276 Bi38 O164 Ti18'
_chemical_formula_sum            'C312 H276 Bi38 O164 Ti18'
_chemical_formula_weight         15452.75
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2022-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   39.6442(16)
_cell_length_b                   39.6442(16)
_cell_length_c                   23.6456(15)
_cell_measurement_reflns_used    12584
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      60.0000
_cell_measurement_theta_min      3.3800
_cell_volume                     32184(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    108.00 142.00   0.40    6.00    --   72.31 111.00 145.00   85
  2  \w      2.00 106.00   0.40    6.00    --   72.31-101.00-104.00  260
  3  \w    -30.00  -4.80   0.40    1.40    --   -1.41 -89.00  26.00   63
  4  \w    -12.00  15.20   0.40    1.40    --   -1.41  89.00 141.00   68
  5  \w     -3.00  21.80   0.40    1.40    --   -1.41 -89.00  26.00   62
  6  \w     80.00 138.00   0.40    6.00    --   72.31 126.00 -27.00  145
  7  \w     58.00 142.00   0.40    6.00    --   72.31  57.00  60.00  210
  8  \w   -142.00-116.80   0.40    6.00    --  -75.13 -99.00   0.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0226975000
_diffrn_orient_matrix_UB_12      -0.0038459000
_diffrn_orient_matrix_UB_13      -0.0385531000
_diffrn_orient_matrix_UB_21      -0.0294366000
_diffrn_orient_matrix_UB_22      -0.0353578000
_diffrn_orient_matrix_UB_23      -0.0138634000
_diffrn_orient_matrix_UB_31      -0.0118159000
_diffrn_orient_matrix_UB_32      0.0161191000
_diffrn_orient_matrix_UB_33      -0.0392239000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33261
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        52.926
_diffrn_reflns_theta_max         52.926
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    23.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull reddish orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_description       cube
_exptl_crystal_F_000             21030
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.816
_refine_diff_density_min         -2.997
_refine_diff_density_rms         0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         12486
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3013
_refine_ls_wR_factor_ref         0.3285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8358
_reflns_number_total             12486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06847d2.cif
_cod_data_source_block           PTC-285
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1566242
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHOTiBi
_shelx_estimated_absorpt_t_max   0.207
_shelx_estimated_absorpt_t_min   0.207
_diffrn_oxdiff_digest_frames
;
01922ad18274439948300934fba3601e2200956c52a
;
_diffrn_oxdiff_digest_hkl
;
016c986132690bc413f464a558355f0ad76125
;
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C106-C8AA
 1.5 with sigma of 0.02
 C8AA-C7AA
 1.5 with sigma of 0.02
 C6AA-C59
 1.5 with sigma of 0.02
 C90-C59
 1.5 with sigma of 0.02
 C51-C67
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O012) = Uanis(C36) = Uanis(C51) = Uanis(C32) = Uanis(C53) = Uanis(C0AA) =
Uanis(C28)
Uanis(O011) = Uanis(C95) = Uanis(C67) = Uanis(C3AA) = Uanis(C137) = Uanis(C156)
= Uanis(C88)
Uanis(C01B) = Uanis(C80) = Uanis(C48) = Uanis(C5AA) = Uanis(C54) = Uanis(C76)
Uanis(C9) = Uanis(C01B)
Uanis(C01E) = Uanis(C01D) = Uanis(C34) = Uanis(C57) = Uanis(C018) = Uanis(C56)
Uanis(C69) = Uanis(C9AA) = Uanis(C58) = Uanis(C1AA) = Uanis(C2AA) = Uanis(C77)
= Uanis(C102)
Uanis(C00Z) = Uanis(C014) = Uanis(C49) = Uanis(C84) = Uanis(C74) = Uanis(C86) =
Uanis(C30)
Uanis(C6AA) = Uanis(C59) = Uanis(C90)
Uanis(C7AA) = Uanis(C8AA) = Uanis(C106)
4.a Riding coordinates:
 C106(H10A,H10B,H10C)
4.b Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C019(H01C,H01D), C01F(H01E,H01F), C12(H12A,H12B), C39(H39A,
 H39B), C42(H42A,H42B), C8AA(H8AA,H8AB), C59(H59A,H59B)
4.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C84(H84), C74(H74), C86(H86), C018(H018), C57(H57), C34(H34),
 C01D(H01G), C137(H137), C3AA(H3AA), C88(H88), C156(H156), C32(H32), C53(H53),
 C0AA(H0AA), C28(H28), C102(H102), C1AA(H1AA), C2AA(H2AA), C77(H77), C80(H80),
 C48(H48), C5AA(H5AA), C54(H54)
4.d Fitted hexagon refined as free rotating group:
 C30(C014,C49,C84,C74,C86), C56(C018,C57,C34,C01D,C01E), C137(C3AA,C95,C67,C88,
 C156), C36(C51,C32,C53,C0AA,C28), C102(C9AA,C58,C1AA,C2AA,C77), C76(C01B,C80,
 C48,C5AA,C54)
4.e Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C)
;
_shelx_res_checksum              2924
_shelx_hkl_checksum              63860
_shelx_fab_checksum              87912
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.444
_oxdiff_exptl_absorpt_empirical_full_min 0.558