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_1566240
_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
'C100 H61 Bi19 O66.5 Ti3, C105 H65 Bi19 O67.5 Ti3'
_chemical_formula_sum            'C254 H244 Bi38 N11 O149 Ti6'
_chemical_formula_weight         14063.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-19
_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                107.5720(10)
_cell_angle_beta                 91.1110(10)
_cell_angle_gamma                114.4930(10)
_cell_formula_units_Z            2
_cell_length_a                   23.6421(2)
_cell_length_b                   23.8375(2)
_cell_length_c                   38.8128(3)
_cell_measurement_reflns_used    113320
_cell_measurement_temperature    100.4(7)
_cell_measurement_theta_max      52.8200
_cell_measurement_theta_min      2.0410
_cell_volume                     18711.2(3)
_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      100.4(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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    -68.00 -33.00   0.50    0.25    --   -1.25 -22.00 -17.00   70
  2  \w     48.00  76.00   0.50    0.87    --   56.89  22.00 148.00   56
  3  \w     96.00 122.00   0.50    0.87    --   56.89  22.00 148.00   52
  4  \w    -16.00  11.00   0.50    0.87    --   56.89 -22.00 -17.00   54
  5  \w    -22.00   5.00   0.50    0.87    --  -59.39  22.00 148.00   54
  6  \w   -135.00 -45.00   0.50    0.87    --  -59.39 -22.00 -17.00  180
  7  \w     15.00  51.00   0.50    0.25    --   -1.25  22.00 148.00   72
  8  \w     -3.00  31.00   0.50    0.25    --   -1.25  57.00-180.00   68
  9  \w    -25.00  14.00   0.50    0.25    --   -1.25 -22.00 -17.00   78
 10  \w    -17.00  43.00   0.50    0.87    --   56.89 -38.00 -60.00  120
 11  \w    -12.00  25.00   0.50    0.87    --   56.89 -19.00-180.00   74
 12  \w     53.00  80.00   0.50    0.87    --   56.89-125.00  60.00   54
 13  \w     20.00  97.00   0.50    0.87    --   56.89-125.00  90.00  154
 14  \w     67.00 128.00   0.50    0.87    --   56.89  57.00  90.00  122
 15  \w   -102.00 -30.00   0.50    0.87    --  -59.39 125.00 120.00  144
 16  \w   -105.00 -70.00   0.50    0.87    --  -59.39 125.00  30.00   70
 17  \w   -105.00 -23.00   0.50    0.87    --  -59.39 125.00-150.00  164
 18  \w    -99.00 -24.00   0.50    0.87    --  -59.39 125.00-180.00  150
 19  \w    -63.00 -13.00   0.50    0.87    --  -59.39  57.00   0.00  100
 20  \w   -128.00 -90.00   0.50    0.87    --  -59.39-125.00  90.00   76
 21  \w    -80.00  12.00   0.50    0.87    --  -59.39  77.00 150.00  184
 22  \w    -26.00  -1.00   0.50    0.87    --  -59.39  19.00 120.00   50
 23  \w    -82.00 -43.00   0.50    0.87    --  -59.39  77.00 -30.00   78
 24  \w    -26.00  16.00   0.50    0.87    --  -59.39  19.00 -60.00   84
;
_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      -0.0362971000
_diffrn_orient_matrix_UB_12      0.0315214000
_diffrn_orient_matrix_UB_13      0.0042611000
_diffrn_orient_matrix_UB_21      0.0516337000
_diffrn_orient_matrix_UB_22      0.0574725000
_diffrn_orient_matrix_UB_23      0.0095828000
_diffrn_orient_matrix_UB_31      -0.0013071000
_diffrn_orient_matrix_UB_32      -0.0038660000
_diffrn_orient_matrix_UB_33      -0.0351759000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            203290
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        52.812
_diffrn_reflns_theta_max         52.812
_diffrn_reflns_theta_min         1.954
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    25.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39698
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.496
_exptl_crystal_description       rodlike
_exptl_crystal_F_000             12646
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.949
_refine_diff_density_min         -8.027
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2989
_refine_ls_number_reflns         64356
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0630P)^2^+215.4900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                51819
_reflns_number_total             64356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06847d2.cif
_cod_data_source_block           PTC-280
_cod_database_code               1566240
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHONTiBi
_diffrn_oxdiff_digest_frames
;
01e6c4316ca86d254103f878df7ba5346a02308c499
;
_diffrn_oxdiff_digest_hkl
;
0129f0a7ccd8fa59496c4d2ef714d21cf84321
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     49.54
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O44-C4BA
 1.3 with sigma of 0.02
 O2DA-C39
 1.3 with sigma of 0.02
 O09M-C39
 1.3 with sigma of 0.02
 C4DA-C39
 1.5 with sigma of 0.02
 C5DA-C05D
 1.5 with sigma of 0.02
 O06O-C5DA
 1.3 with sigma of 0.02
 C71-C60
 1.45 with sigma of 0.02
 O02S-C05G
 1.3 with sigma of 0.02
 C06M-C072
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C069 \\sim O06Q \\sim C09F \\sim O05W: within 3.8A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C39 \\sim O09M \\sim O2DA \\sim C4DA: within 3.8A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C36 \\sim C9AA \\sim C68 \\sim C08K: within 3.8A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C39 \\sim C4DA \\sim O2DA \\sim O09M: within 3.8A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C069 \\sim O06Q \\sim O05W \\sim C09F: within 3.8A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C39 \\sim O2DA \\sim C4DA \\sim O09M: within 3.8A with sigma of 0.004 and sigma
for terminal atoms of 0.008
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O09L) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O03F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2DA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O09M) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C127) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O09M) \\sim Ueq, Uanis(O09H) \\sim Ueq, : with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uiso(C09F) = Uiso(C97) = Uiso(C498) = Uiso(C178) = Uiso(C146) = Uiso(C115)
Uiso(C4BA) = Uiso(C118) = Uiso(C117) = Uiso(C197) = Uiso(C3BA) = Uiso(C05D)
Uiso(C06M) = Uiso(C05N) = Uiso(C162) = Uiso(C155) = Uiso(C108) = Uiso(C114)
Uiso(C072) = Uiso(O05Q) = Uiso(O37)
Uiso(O06O) = Uiso(C5DA) = Uiso(O06O) = Uiso(O07T)
Uanis(C60) = Uanis(C112) = Uanis(C130) = Uanis(C0BA) = Uanis(C0AA) = Uanis(C122)
Uanis(C36) = Uanis(C68) = Uanis(C127) = Uanis(C8AA) = Uanis(C88) = Uanis(C9AA)
Uanis(C055) = Uanis(C161) = Uanis(C160) = Uanis(C150) = Uanis(C134) =
Uanis(C5CA)
4.a Aromatic/amide H refined with riding coordinates:
 C04J(H04J), C04Y(H04Y), C051(H051), C118(H118), C117(H117), C3BA(H3BA),
 C197(H197), C05H(H05H), C05J(H05J), C05K(H05K), C05L(H05L), C05T(H05T),
 C05U(H05U), C05X(H05X), C05Y(H05Y), C064(H064), C068(H068), C06A(H06A),
 C06C(H06C), C06I(H06I), C06J(H06J), C06K(H06K), C06L(H06L), C05N(H05N),
 C162(H162), C155(H155), C108(H108), C06T(H06T), C070(H070), C073(H073),
 C074(H074), C075(H075), C076(H076), C07A(H07A), C07B(H07B), C07O(H07O),
 C07P(H07P), C07Q(H07Q), C07S(H07S), C07U(H07U), C07X(H07X), C07Y(H07Y),
 C07Z(H07Z), C081(H081), C083(H083), C086(H086), C08F(H08F), C08G(H08G),
 C08L(H08L), C08N(H08N), C08X(H08X), C08Y(H08Y), C091(H091), C099(H099),
 C9BA(H9BA), C09C(H09C), C48(H48), C93(H93), C100(H100), C43(H43), C09I(H09I),
 C4CA(H4CA), C46(H46), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C61(H61), C63(H63), C65(H65), C72(H72), C76(H76), C78(H78), C79(H79),
  C80(H80), C81(H81), C83(H83), C134(H134), C150(H150), C160(H160), C161(H161),
 C91(H91), C95(H95), C98(H98), C99(H99), C101(H101), C103(H103), C106(H106),
 C128(H128), C09G(H09G), C107(H107), C109(H109), C86(H86), C124(H124),
 C126(H126), C110(H110), C122(H122), C0AA(H0AA), C0BA(H0BA), C130(H130),
 C113(H113), C138(H138), C144(H144), C173(H173), C8AA(H8AA), C88(H88),
 C9AA(H9AA), C127(H127), C0CA(H0CA), C1CA(H1CA), C498(H498), C178(H178),
 C146(H146), C97(H97)
4.b Fitted hexagon refined as free rotating group:
 C05D(C4BA,C118,C117,C3BA,C197), C06M(C05N,C162,C155,C108,C114), C09E(C08T,C48,
 C93,C100,C43), C5CA(C134,C150,C160,C161,C055), C103(C106,C128,C09G,C06Y,C098),
 C109(C41,C077,C86,C124,C126), C112(C60,C122,C0AA,C0BA,C130), C8AA(C88,C9AA,C36,
 C68,C127), C498(C178,C146,C115,C09F,C97)
4.c Tetrahedral OH refined with riding coordinates:
 O05Z(H05Z), O49(H49), O84(H84), O0AA(H0AB), O44(H44)
4.d Idealised tetrahedral OH refined as rotating group:
 O033(H033), O04C(H04C), O04S(H04S), O07C(H07C), O08M(H08M)
;
_shelx_res_checksum              58138
_shelx_hkl_checksum              85595
_shelx_fab_checksum              28070
_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 11.074
_oxdiff_exptl_absorpt_empirical_full_min 0.315