Designed sol-gel precursors for atomically dispersed Nb and Pb within TiO<sub>2</sub> as catalysts for dihydroxyacetone transformation.
Neto, Antonio de Brito Santiago; Alves da Cruz, Márcia Gabriely; Jeanneau, Erwann; Oliveira, Alcineia Conceição; Essayem, Nadine; Mishra, Shashank; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1604–1609; doi:10.1039/d0dt03726e

data_7706426
_publ_section_title
;
 Designed sol-gel precursors for atomically dispersed Nb and Pb within
 TiO<sub>2</sub> as catalysts for dihydroxyacetone transformation.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1604
_journal_page_last               1609
_journal_paper_doi               10.1039/d0dt03726e
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C12 H27 N2 Nb2 O8'
_chemical_formula_sum            'C12 H27 N2 Nb2 O8'
_chemical_formula_weight         513.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-09-30 deposited with the CCDC.	2021-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.473(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8106(13)
_cell_length_b                   10.2674(13)
_cell_length_c                   18.4561(18)
_cell_measurement_reflns_used    7625
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2260
_cell_measurement_theta_min      3.3870
_cell_volume                     2327.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.906
_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    -38.00  63.00   1.00   42.24    --  -10.24  57.00-180.00  101
  2  \w    -51.00  70.00   1.00   42.24    --  -10.24  19.00 -60.00  121
  3  \w    -21.00  39.00   1.00   42.24    --   11.34  77.00  90.00   60
  4  \w    -85.00  14.00   1.00   42.24    --  -10.24 -37.00 150.00   99
  5  \w    -21.00  39.00   1.00   42.24    --   11.34  77.00 -30.00   60
  6  \w    -18.00   7.00   1.00   42.24    --   11.34 -77.00 -60.00   25
  7  \w    -13.00  47.00   1.00   42.24    --   11.34 -88.00  71.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0063029000
_diffrn_orient_matrix_UB_12      -0.0395880000
_diffrn_orient_matrix_UB_13      0.0299691000
_diffrn_orient_matrix_UB_21      -0.0348082000
_diffrn_orient_matrix_UB_22      0.0474699000
_diffrn_orient_matrix_UB_23      0.0086589000
_diffrn_orient_matrix_UB_31      -0.0455692000
_diffrn_orient_matrix_UB_32      -0.0309513000
_diffrn_orient_matrix_UB_33      -0.0251867000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16317
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.610
_diffrn_reflns_theta_min         3.134
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.168
_refine_diff_density_max         3.208
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5581
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1415P)^2^+15.8238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2488
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                4310
_reflns_number_total             5581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03726e2.cif
_cod_data_source_block           smr-b-xxx
_cod_depositor_comments
'Adding full bibliography for 7706424--7706426.cif.'
_cod_database_code               7706426
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H56 N4 Nb4 O16'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(13)
 0.49(13)
2. 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
3. Restrained distances
 C8-C7
 2.6 with sigma of 0.04
 N1-C5 \\sim N1-C3 \\sim N1-C2 \\sim N2-C8 \\sim N2-C7 \\sim N2-C10
 with sigma of 0.02
 C10-C11 \\sim C9-C8 \\sim C2-C1 \\sim C3-C4
 with sigma of 0.02
 O7-C11 \\sim O5-C9 \\sim O3-C1 \\sim O2-C4 \\sim O4-C6 \\sim O6-C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim
C7 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Nb1 \\sim Nb2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
5. Rigid body (RIGU) restrains
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C4, C5, C6, C7, C10,
  C11, C12
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C4, C5, C6, C7, C8,
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
 Nb1, Nb2, O1, O2, O3, O4, O5, O6, O7, O8, N1, N2, C1, C2, C3, C4, C5, C6, C7,
 C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2020-09-24
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id SMR-b-XXX
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.812