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_1566244
_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         'C300 H290 Bi38 N2 O184 Ti20, 2(C3 H7 N O)'
_chemical_formula_sum            'C306 H304 Bi38 N4 O186 Ti20'
_chemical_formula_weight         15912.75
_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             2021-08-20
_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                117.688(2)
_cell_angle_beta                 115.545(2)
_cell_angle_gamma                92.2502(17)
_cell_formula_units_Z            1
_cell_length_a                   23.1533(5)
_cell_length_b                   23.5480(5)
_cell_length_c                   23.6018(5)
_cell_measurement_reflns_used    47313
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      60.5460
_cell_measurement_theta_min      2.2140
_cell_volume                     9807.3(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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      9.00  63.00   0.50    0.36    --   72.34 -57.00  90.00  108
  2  \w      0.00  95.00   0.50    0.36    --   72.34 -77.00  90.00  190
  3  \w      6.00  66.00   0.50    0.36    --   72.34 -57.00   0.00  120
  4  \w     -2.00  24.00   0.50    0.36    --   72.34 -19.00 120.00   52
  5  \w     89.00 132.00   0.50    0.36    --   72.34  98.00  31.00   86
  6  \w      4.00  39.00   0.50    0.36    --   72.34 -38.00 -60.00   70
  7  \w     -1.00  26.00   0.50    0.36    --   72.34 -19.00 -30.00   54
  8  \w     37.00  83.00   0.50    0.36    --   72.34 -98.00 -75.00   92
  9  \w     77.00 111.00   0.50    0.36    --   72.34-125.00-150.00   68
 10  \w     21.00  46.00   0.50    0.36    --   72.34-125.00-150.00   50
 11  \w     62.00 109.00   0.50    0.36    --   72.34-125.00 -60.00   94
 12  \w     55.00 102.00   0.50    0.36    --   72.34-125.00  90.00   94
 13  \w   -140.00 -89.00   0.50    0.36    --  -75.15 -98.00 -75.00  102
 14  \w   -146.00-120.00   0.50    0.36    --  -75.15-125.00-150.00   52
 15  \w   -110.00 -82.00   0.50    0.36    --  -75.15-125.00-150.00   56
 16  \w    -76.00  14.00   0.50    0.09    --   -1.41 -19.00 -30.00  180
 17  \w    -30.00  14.00   0.50    0.09    --   -1.41 -77.00 -90.00   88
 18  \w    -73.00 -35.00   0.50    0.09    --   -1.41 -77.00 -90.00   76
 19  \w    -56.00  -7.00   0.50    0.36    --  -75.15  57.00-150.00   98
 20  \w    -65.00  -3.00   0.50    0.36    --  -75.15  57.00-120.00  124
 21  \w    -65.00  -8.00   0.50    0.36    --  -75.15  57.00   0.00  114
 22  \w    -40.00  -7.00   0.50    0.36    --  -75.15  38.00 -30.00   66
 23  \w    -41.00  -3.00   0.50    0.36    --  -75.15  38.00 -60.00   76
 24  \w    -33.00  -4.00   0.50    0.36    --  -75.15  38.00-180.00   58
 25  \w    -41.00  -5.00   0.50    0.36    --  -75.15  38.00  60.00   72
 26  \w    -30.00  -4.00   0.50    0.36    --  -75.15  38.00 150.00   52
 27  \w    -15.00  15.00   0.50    0.09    --   -1.41  38.00 150.00   60
 28  \w     25.00  72.00   0.50    0.09    --   -1.41  38.00 150.00   94
 29  \w    -26.00  -1.00   0.50    0.36    --  -75.15  19.00   0.00   50
 30  \w    -26.00  -1.00   0.50    0.36    --  -75.15  19.00  30.00   50
 31  \w    -26.00  -1.00   0.50    0.36    --  -75.15  19.00 -30.00   50
 32  \w    -25.00   0.00   0.50    0.36    --  -75.15  19.00 -60.00   50
 33  \w    -30.00  -2.00   0.50    0.36    --  -75.15  38.00-120.00   56
 34  \w    -35.00 -10.00   0.50    0.09    --   -1.41  98.00  31.00   50
 35  \w    -98.00 -59.00   0.50    0.36    --  -75.15 125.00 150.00   78
 36  \w   -104.00 -46.00   0.50    0.36    --  -75.15  98.00  31.00  116
;
_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      0.0590035000
_diffrn_orient_matrix_UB_12      0.0117115000
_diffrn_orient_matrix_UB_13      0.0037609000
_diffrn_orient_matrix_UB_21      -0.0234654000
_diffrn_orient_matrix_UB_22      -0.0581154000
_diffrn_orient_matrix_UB_23      -0.0649467000
_diffrn_orient_matrix_UB_31      -0.0219559000
_diffrn_orient_matrix_UB_32      0.0319317000
_diffrn_orient_matrix_UB_33      -0.0359454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            120835
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        52.928
_diffrn_reflns_theta_max         52.928
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    25.420
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37182
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_description       block
_exptl_crystal_F_000             7250
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.540
_refine_diff_density_min         -3.341
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2394
_refine_ls_number_reflns         34316
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0950P)^2^+327.8800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25053
_reflns_number_total             34316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06847d2.cif
_cod_data_source_block           PTC-286
_cod_original_cell_volume        9807.4(4)
_cod_database_code               1566244
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHONTiBi
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.185
_diffrn_oxdiff_digest_frames
;
016bb29ea69d8b2092a40d2c8a0b84c0360294644e7
;
_diffrn_oxdiff_digest_hkl
;
01881f8026e49333cfb3b4caccdb44486cb08b
;
_reflns_odcompleteness_completeness 98.70
_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
 O069-C120
 1.5 with sigma of 0.02
 C48-C106
 1.5 with sigma of 0.02
 N05M-C66 = N05M-C20
 1.5 with sigma of 0.02
 O02C-C044
 1.4 with sigma of 0.02
 C04K-C047
 1.5 with sigma of 0.02
 C69-C29
 1.5 with sigma of 0.02
 O039-C36
 1.45 with sigma of 0.02
 C05K-C04H
 1.5 with sigma of 0.02
 O02J-C04H
 1.3 with sigma of 0.02
 O050-C75
 1.5 with sigma of 0.02
 O04Q-C04A
 1.3 with sigma of 0.02
 O02G-C04A
 1.3 with sigma of 0.02
 Ti00-O069 = Ti00-O050
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C04H) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C04Y) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C04A) \\sim Ueq, Uanis(C05H) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O069) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C90) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C04A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C03F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C52) = Uanis(C41) = Uanis(C42) = Uanis(C28) = Uanis(C45) = Uanis(C79) =
Uanis(C178)
Uanis(O039) = Uanis(C36)
Uanis(C162) = Uanis(C48) = Uanis(C106)
Uanis(C17) = Uanis(C29) = Uanis(C69)
4.a Secondary CH2 refined with riding coordinates:
 C037(H03A,H03B), C03A(H03C,H03D), C03F(H03H,H03I), C03I(H03J,H03K), C048(H04D,
 H04E), C04C(H04G,H04H), C04E(H04J,H04K), C04F(H04L,H04M), C04K(H04O,H04P),
 C04O(H04Q,H04R), C04U(H04S,H04T), C04W(H04U,H04V), C054(H05A,H05B), C05A(H05C,
 H05D), C05C(H05E,H05F), C05E(H05H,H05I), C05H(H05K,H05L), C05R(H05Q,H05R),
 C4(H4A,H4B), C23(H23A,H23B), C29(H29A,H29B), C31(H31A,H31B), C48(H48A,H48B),
 C27(H27A,H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C03B(H03E), C03C(H03F), C03E(H03G), C03K(H03L), C03L(H03M), C03Q(H03Q),
 C03T(H03T), C03V(H03V), C03W(H03W), C03X(H03X), C040(H040), C041(H041),
 C043(H043), C044(H044), C046(H046), C04B(H04F), C04D(H04I), C04J(H04N),
 C04X(H04X), C052(H052), C058(H058), C059(H059), C05D(H05G), C05G(H05J),
 C05J(H05M), C05L(H05N), C05N(H05O), C05O(H05P), C05T(H05T), C05U(H05U),
 C05Z(H05Z), C060(H060), C061(H061), C062(H062), C063(H063), C066(H066),
 C06E(H06E), C06H(H06H), C9(H9), C19(H19), C54(H54), C90(H90), C70(H70),
 C06I(H06I), C61(H61), C06F(H06F), C06B(H06D), C64(H64), C65(H65), C72(H72),
 C065(H065), C04T(H04W), C68(H68), C84(H84), C178(H178), C79(H79), C45(H45),
 C28(H28), C0AA(H0AA), C50(H50), C51(H51), C2AA(H2AA)
4.c Fitted hexagon refined as free rotating group:
 C44(C58,C54,C90,C70,C06I), C61(C05P,C06C,C06F,C06B,C64), C72(C065,C05I,C042,
 C04T,C68), C178(C79,C45,C28,C42,C41)
4.d Idealised Me refined as rotating group:
 C03P(H03N,H03O,H03P), C047(H04A,H04B,H04C), C06A(H06A,H06B,H06C), C8(H8A,H8B,
 H8C), C69(H69A,H69B,H69C), C106(H10A,H10B,H10C), C36(H36A,H36B,H36C), C46(H46A,
 H46B,H46C), C1AA(H1AA,H1AB,H1AC), C43(H43A,H43B,H43C), C39(H39A,H39B,H39C),
 C57(H57A,H57B,H57C), C20(H20A,H20B,H20C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              86166
_shelx_hkl_checksum              68393
_shelx_fab_checksum              54919
_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 2.084
_oxdiff_exptl_absorpt_empirical_full_min 0.550