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_7706425
_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_formula_moiety         'C10 H20 N2 O4 Pb2'
_chemical_formula_sum            'C10 H20 N2 O4 Pb2'
_chemical_formula_weight         646.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-01 deposited with the CCDC.	2021-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.767(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.674(3)
_cell_length_b                   10.4513(13)
_cell_length_c                   22.478(3)
_cell_measurement_reflns_used    5417
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.2820
_cell_measurement_theta_min      3.8010
_cell_volume                     3708.9(10)
_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 0.885
_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    -41.00  62.00   1.00   10.00    --  -11.61  57.00 -90.00  103
  2  \w   -100.00 -32.00   1.00   10.00    --  -11.61 178.00-120.00   68
  3  \w    -75.00  20.00   1.00   10.00    --  -11.61 -77.00 -90.00   95
  4  \w    -83.00   9.00   1.00   10.00    --  -11.61 -57.00 120.00   92
;
_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      -0.0027279000
_diffrn_orient_matrix_UB_12      0.0676550000
_diffrn_orient_matrix_UB_13      -0.0017408000
_diffrn_orient_matrix_UB_21      0.0341330000
_diffrn_orient_matrix_UB_22      0.0044963000
_diffrn_orient_matrix_UB_23      0.0285578000
_diffrn_orient_matrix_UB_31      0.0290236000
_diffrn_orient_matrix_UB_32      0.0008736000
_diffrn_orient_matrix_UB_33      -0.0171845000
_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  0.0631
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16609
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_min         3.274
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.139
_exptl_absorpt_correction_T_max  0.083
_exptl_absorpt_correction_T_min  0.021
_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    2.316
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.214
_refine_diff_density_max         2.633
_refine_diff_density_min         -2.662
_refine_diff_density_rms         0.350
_refine_ls_extinction_coef       0.00034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0652P)^2^+41.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3790
_reflns_number_total             4637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03726e2.cif
_cod_data_source_block           smrb101_4
_cod_depositor_comments
'Adding full bibliography for 7706424--7706426.cif.'
_cod_original_cell_volume        3709.0(9)
_cod_database_code               7706425
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C5 H10 N1 O2 Pb1'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93564
_shelx_fab_checksum              86732
_olex2_date_sample_data_collection 2016-05-11
_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 smeb101_4
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.668