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_1566241
_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         'C234 H180 Bi38 O152 Ti14'
_chemical_formula_sum            'C252 H222 Bi38 N6 O158 Ti14'
_chemical_formula_weight         14474.18
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-08-20
_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            6
_cell_length_a                   24.8265(5)
_cell_length_b                   24.8265(5)
_cell_length_c                   120.4773(15)
_cell_measurement_reflns_used    25556
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      60.5590
_cell_measurement_theta_min      2.2060
_cell_volume                     64308(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -43.00  -1.90   0.15    0.21    --  -75.15  77.00 -30.00  274
  2  \w    -30.00  -3.00   0.15    0.21    --  -75.15  38.00 -60.00  180
  3  \w    -26.00  -0.95   0.15    0.21    --  -75.15  19.00 -30.00  167
  4  \w    -42.00  -3.00   0.15    0.21    --  -75.15  38.00 -90.00  260
  5  \w    -39.10  -1.00   0.15    0.21    --  -75.15  38.00 -30.00  254
  6  \w    -71.00 -36.05   0.15    0.05    --   -1.41 -38.00-180.00  233
  7  \w    -27.00   2.10   0.15    0.05    --   -1.41 -38.00-180.00  194
  8  \w    -97.00 -59.95   0.15    0.21    --  -75.15  77.00 -30.00  247
  9  \w   -144.00-112.95   0.15    0.21    --  -75.15-111.00 141.00  207
 10  \w   -146.00-101.00   0.15    0.21    --  -75.15-143.00 101.00  300
 11  \w     95.00 125.00   0.15    0.21    --   72.34 111.00-125.00  200
;
_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      -0.0205816667
_diffrn_orient_matrix_UB_12      0.0398006667
_diffrn_orient_matrix_UB_13      -0.0018506333
_diffrn_orient_matrix_UB_21      -0.0566952000
_diffrn_orient_matrix_UB_22      -0.0477483000
_diffrn_orient_matrix_UB_23      -0.0023244000
_diffrn_orient_matrix_UB_31      -0.0157895667
_diffrn_orient_matrix_UB_32      -0.0033560333
_diffrn_orient_matrix_UB_33      0.0107056667
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       143
_diffrn_reflns_limit_l_min       -83
_diffrn_reflns_number            67131
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        52.927
_diffrn_reflns_theta_max         52.927
_diffrn_reflns_theta_min         2.195
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    22.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_description       block
_exptl_crystal_F_000             39012
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.268
_refine_diff_density_min         -3.469
_refine_diff_density_rms         0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         12593
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0831
_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^)+(0.1236P)^2^+4539.6250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9994
_reflns_number_total             12593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06847d2.cif
_cod_data_source_block           PTC-282
_cod_original_cell_volume        64308(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               1566241
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHONTiBi
_shelx_estimated_absorpt_t_max   0.211
_shelx_estimated_absorpt_t_min   0.093
_diffrn_oxdiff_digest_frames
;
01eecc7579c6dbdc2ccbc174198ce763d502516f8d8
;
_diffrn_oxdiff_digest_hkl
;
011c611f5d0963d3791e8debdc43f55d007cd4
;
_reflns_odcompleteness_completeness 99.64
_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
 O00Q-C018
 1.5 with sigma of 0.02
 O00Y-C0BA
 1.5 with sigma of 0.02
 C131-C0BA
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8AA \\sim C017 \\sim O00W: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C6AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C017) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O00Y) = Uanis(C0BA) = Uanis(C131)
Uanis(C13) = Uanis(C7AA) = Uanis(C1BA)
Uanis(C014) = Uanis(C013) = Uanis(C16) = Uanis(C4AA) = Uanis(C1AA) = Uanis(C2AA)
Uanis(C12) = Uanis(C17) = Uanis(C14) = Uanis(C79) = Uanis(C56) = Uanis(C35)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C0BA(H0BA,H0BB)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C4AA(H4AA), C1AA(H1AA), C2AA(H2AA), C017(H017), C9AA(H9AA),
 C6AA(H6AA), C18(H18), C019(H019), C15(H15), C01F(H01F), C3AA(H3AA), C0AA(H0AA),
  C14(H14), C79(H79), C56(H56), C35(H35), C7AA(H7AA), C1BA(H1BA), C102(H102)
4.c Fitted hexagon refined as free rotating group:
 C014(C013,C16,C4AA,C1AA,C2AA), C01A(C8,C9AA,C6AA,C18,C019), C15(C01B,C01E,
 C01F,C3AA,C0AA), C12(C17,C14,C79,C56,C35)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C131(H13A,H13B,H13C)
;
_shelx_res_checksum              24692
_shelx_hkl_checksum              13241
_shelx_fab_checksum              19305
_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 2.925
_oxdiff_exptl_absorpt_empirical_full_min 0.607