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_1566243
_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         'C210 H132 Bi38 O135 Ti6, 10(C3 H7 N O)'
_chemical_formula_sum            'C240 H202 Bi38 N10 O145 Ti6'
_chemical_formula_weight         13774.74
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-01
_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                 91.5690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6643(3)
_cell_length_b                   33.3838(3)
_cell_length_c                   35.4595(3)
_cell_measurement_reflns_used    74769
_cell_measurement_temperature    104.2(3)
_cell_measurement_theta_max      60.5800
_cell_measurement_theta_min      2.5300
_cell_volume                     37469.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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      104.2(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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     25.00  51.00   0.50    0.05    --   -1.56  57.00-115.00   52
  2  \w    -14.00  67.00   0.50    0.05    --   -1.56  38.00-150.00  162
  3  \w     77.00 143.00   0.50    0.17    --   72.34  57.00-115.00  132
  4  \w     81.00 142.00   0.50    0.17    --   72.34 125.00  90.00  122
  5  \w      0.00  62.00   0.50    0.17    --   72.34 -57.00 103.00  124
  6  \w     -2.00  23.00   0.50    0.17    --   72.34 -19.00 150.00   50
  7  \w      0.00  43.00   0.50    0.17    --   72.34 -38.00 150.00   86
  8  \w     -3.00  25.00   0.50    0.17    --   72.34 -19.00   0.00   56
  9  \w     -1.00  25.00   0.50    0.17    --   72.34 -38.00 -90.00   52
 10  \w    -73.00 -33.00   0.50    0.05    --   -1.56 -57.00 103.00   80
 11  \w    -90.00 -65.00   0.50    0.17    --  -75.46 -57.00 103.00   50
 12  \w    -26.00  -1.00   0.50    0.17    --  -75.46  19.00   0.00   50
 13  \w    -25.00   0.00   0.50    0.17    --  -75.46  19.00 -30.00   50
 14  \w    -42.00  -2.00   0.50    0.17    --  -75.46  38.00  30.00   80
 15  \w    -26.00   0.00   0.50    0.17    --  -75.46  19.00  90.00   52
 16  \w    -30.00  -5.00   0.50    0.17    --  -75.46  38.00  60.00   50
 17  \w    -39.00 -14.00   0.50    0.17    --  -75.46  38.00   0.00   50
 18  \w    -55.00  -5.00   0.50    0.17    --  -75.46  57.00  30.00  100
 19  \w    -63.00  -3.00   0.50    0.17    --  -75.46  57.00-115.00  120
 20  \w    -62.00  -6.00   0.50    0.17    --  -75.46  57.00-180.00  112
;
_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      0.0045381000
_diffrn_orient_matrix_UB_12      0.0271614000
_diffrn_orient_matrix_UB_13      0.0276079000
_diffrn_orient_matrix_UB_21      0.0420484000
_diffrn_orient_matrix_UB_22      -0.0027572000
_diffrn_orient_matrix_UB_23      -0.0020889000
_diffrn_orient_matrix_UB_31      -0.0002619000
_diffrn_orient_matrix_UB_32      0.0294352000
_diffrn_orient_matrix_UB_33      -0.0256829000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            139873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.909
_diffrn_reflns_theta_min         2.711
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    24.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.442
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             24632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         10.941
_refine_diff_density_min         -8.353
_refine_diff_density_rms         0.607
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1840
_refine_ls_number_reflns         38190
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1890P)^2^+555.5760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32395
_reflns_number_total             38190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06847d2.cif
_cod_data_source_block           PTC-280R
_cod_database_code               1566243
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O N Ti Bi'
_diffrn_oxdiff_digest_frames
;
019662b67d574167ad13547379fda1f311016308116
;
_diffrn_oxdiff_digest_hkl
;
01c84df4b91ee8b7e70ba85aa8e3e09c324581
;
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_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, All O(H) groups
2. Restrained distances
 O01T-H01T
 0.85 with sigma of 0.01
 C02T-H01T
 1.845617 with sigma of 0.02
 Ti0K-H01T
 2.486344 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C03S \\sim O98 \\sim O02A \\sim C42: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C3BA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O98) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C90) = Uanis(C61)
Uanis(N51) = Uanis(C98)
Uanis(C42) = Uanis(C5CA) = Uanis(C1EA) = Uanis(C240) = Uanis(C7DA) = Uanis(C6CA)
Uanis(C03K) = Uanis(C7BA) = Uanis(C152) = Uanis(C7CA) = Uanis(C113) =
Uanis(C86) = Uanis(C5DA)
Uanis(C58) = Uanis(C108) = Uanis(C96) = Uanis(C8CA) = Uanis(C4DA) = Uanis(C97)
4.a Aromatic/amide H refined with riding coordinates:
 C02U(H02U), C02V(H02V), C2BA(H2BA), C1BA(H1BA), C92(H92), C3BA(H3BA),
 C03G(H03G), C042(H042), C04B(H04B), C04H(H04H), C04P(H04P), C04S(H04S),
 C04T(H04T), C04U(H04U), C05K(H05K), C065(H065), C06G(H06G), C06K(H06K),
 C49(H49), C57(H57), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
  C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80),
 C85(H85), C88(H88), C90(H90), C97(H97), C96(H96), C8CA(H8CA), C4DA(H4DA),
 C99(H99), C1AA(H1AA), C56(H56), C9AA(H9AA), C4AA(H4AA), C0BA(H0BA), C82(H82),
 C0AA(H0AA), C5AA(H5AA), C7AA(H7AA), C5BA(H5BA), C5CA(H5CA), C1EA(H1EA),
 C240(H240), C7DA(H7DA), C0CA(H0CA), C87(H87), C152(H152), C7CA(H7CA),
 C113(H113), C5DA(H5DA), C6BA(H6BA), C3DA(H3DA), C9DA(H9DA), C9CA(H9CA)
4.b Fitted hexagon refined as free rotating group:
 C038(C2BA,C1BA,C92,C3BA,C4CA), C97(C58,C108,C96,C8CA,C4DA), C42(C5CA,C1EA,
 C240,C7DA,C6CA), C7BA(C152,C7CA,C113,C5DA,C86)
4.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C93(H93A,H93B,H93C), C100(H10A,H10B,H10C), C2AA(H2AA,
 H2AB,H2AC), C3AA(H3AA,H3AB,H3AC), C4BA(H4BA,H4BB,H4BC), C1DA(H1DA,H1DB,H1DC),
 C0DA(H0DA,H0DB,H0DC), C0EA(H0EA,H0EB,H0EC), C98(H98A,H98B,H98C)
4.d Idealised tetrahedral OH refined as rotating group:
 O02O(H02O), O034(H034), O71(H71), O45(H45), O2DA(H2DA)
;
_shelx_res_checksum              67516
_shelx_hkl_checksum              59506
_shelx_fab_checksum              18212
_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 3.282
_oxdiff_exptl_absorpt_empirical_full_min 0.423