A scandium-containing polyoxoniobate heptamer as a catalyst for the Knoevenagel condensation reaction.
Lin, Ya-Ting; Zeng, Li; Li, Yi-Ying; Sun, Yan-Qiong; Li, Xin-Xiong; Zheng, Shou-Tian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8425–8429; doi:10.1039/d5dt00569h

data_7718596
_publ_section_title
;
 A scandium-containing polyoxoniobate heptamer as a catalyst for the
 Knoevenagel condensation reaction.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8425
_journal_page_last               8429
_journal_paper_doi               10.1039/d5dt00569h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'K10 Na21 Nb49 O199 Sc3, 71[H2O]'
_chemical_formula_sum            'K9 Na16.5 Nb49 O192.5 Sc3'
_chemical_formula_weight         8498.71
_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_primary     iterative
_audit_creation_date             2025-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-17 deposited with the CCDC.	2025-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.906(2)
_cell_angle_beta                 102.223(2)
_cell_angle_gamma                107.8870(10)
_cell_formula_units_Z            2
_cell_length_a                   18.6202(16)
_cell_length_b                   19.6569(16)
_cell_length_c                   38.958(3)
_cell_measurement_reflns_used    9119
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.994
_cell_measurement_theta_min      2.534
_cell_volume                     13044.4(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            194902
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.034
_diffrn_reflns_theta_max         25.034
_diffrn_reflns_theta_min         1.798
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0377 after correction.
The Ratio of minimum to maximum transmission is 0.8183.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7929
_exptl_crystal_recrystallization_method
'The crystals were growth by means of evaporation of a mixture of n-hexane and toluene at RT.'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.184
_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2843
_refine_ls_number_reflns         44336
_refine_ls_number_restraints     1405
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.105
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+165.2048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                39877
_reflns_number_total             44336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00569h2.cif
_cod_data_source_block           sc-nb
_cod_depositor_comments          'Adding full bibliography for 7718596.cif.'
_cod_original_cell_volume        13044.3(19)
_cod_original_formula_sum        'K9 Na16.50 Nb49 O192.50 Sc3'
_cod_database_code               7718596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.746
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately
 coated with polybutenes oil (CAS: 9003-29-6) on a glass slide.
 A suitable single crystal coated with polybutenes oil as less as possible
 was sealed in capillary tube filled with argon. The capillary tube with
 single crystal was mounted on copper pin with solid paraffin.
;
_olex2_refinement_description
;
1. Restrained distances
 Na16-O185 \\sim Na16-O200
 with sigma of 0.02
 O15W-Na8A \\sim O15X-Na8A
 with sigma of 0.02
 Na7-O15W \\sim Na7-O15X
 with sigma of 0.02
 Na8B-O15W \\sim Na8B-O15X
 with sigma of 0.02
 K4-O15W \\sim K4-O15X
 with sigma of 0.02
 K4A-O15W \\sim K4A-O15X
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O177 \\sim O185 \\sim O200: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
O20B \\sim O24B \\sim O24A \\sim O158 \\sim O182 \\sim O20C \\sim O35 \\sim O49
\\sim O44 \\sim O180: within 3A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 3A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O20 \\sim Nb1A \\sim Nb2A \\sim Nb3A \\sim Nb4A \\sim Nb5A
\\sim Nb6A \\sim Nb7A \\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim
O6A \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim O11A \\sim O12A \\sim O13A
\\sim O14A \\sim O15A \\sim O16A \\sim O17A \\sim O18A \\sim O20A \\sim Nb8
\\sim Nb9 \\sim Nb10 \\sim Nb11 \\sim Nb12 \\sim Nb13 \\sim Nb14 \\sim Nb15
\\sim Nb16 \\sim Nb17 \\sim Nb18 \\sim Nb19 \\sim Nb20 \\sim Nb21 \\sim Nb22
\\sim Nb23 \\sim Nb24 \\sim Nb25 \\sim Nb26 \\sim Nb27 \\sim Nb28 \\sim Nb29
\\sim Nb30 \\sim Nb31 \\sim Nb32 \\sim Nb33 \\sim Nb34 \\sim Nb35 \\sim Nb36
\\sim Nb37 \\sim Nb38 \\sim Nb39 \\sim Nb40 \\sim Nb41 \\sim Nb42 \\sim Nb43
\\sim Nb44 \\sim Nb45 \\sim Nb46 \\sim Nb47 \\sim Nb48 \\sim Nb49 \\sim O19
\\sim O20B \\sim O20C \\sim O21 \\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim
O5A \\sim O6A \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim O11A \\sim O12A
\\sim O13A \\sim O14A \\sim O15A \\sim O16A \\sim O17A \\sim O18A \\sim O20A
\\sim Nb8 \\sim Nb9 \\sim Nb10 \\sim Nb11 \\sim Nb12 \\sim Nb13 \\sim Nb14
\\sim Nb15 \\sim Nb16 \\sim Nb17 \\sim Nb18 \\sim Nb19 \\sim Nb20 \\sim Nb21
\\sim Nb22 \\sim Nb23 \\sim Nb24 \\sim Nb25 \\sim Nb26 \\sim Nb27 \\sim Nb28
\\sim Nb29 \\sim Nb30 \\sim Nb31 \\sim Nb32 \\sim Nb33 \\sim Nb34 \\sim Nb35
\\sim Nb36 \\sim Nb37 \\sim Nb38 \\sim Nb39 \\sim Nb40 \\sim Nb41 \\sim Nb42
\\sim Nb43 \\sim Nb44 \\sim Nb45 \\sim Nb46 \\sim Nb47 \\sim Nb48 \\sim Nb49
\\sim O19 \\sim O20B \\sim O20C \\sim O21 \\sim O22 \\sim O154 \\sim O23 \\sim
O23A \\sim O24 \\sim O24A \\sim O24B \\sim O25 \\sim O26 \\sim O27 \\sim O28
\\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36
\\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44
\\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49 \\sim O50 \\sim O51 \\sim O52
\\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim O57 \\sim O58 \\sim O59 \\sim O60
\\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim O65 \\sim O66 \\sim O67 \\sim O68
\\sim O69 \\sim O70 \\sim O71 \\sim O72 \\sim O73 \\sim O74 \\sim O75 \\sim O76
\\sim O77 \\sim O78 \\sim O79 \\sim O80 \\sim O81 \\sim O82 \\sim O83 \\sim O84
\\sim O85 \\sim O86 \\sim O87 \\sim O88 \\sim O89 \\sim O90 \\sim O91 \\sim O92
\\sim O93 \\sim O94 \\sim O95 \\sim O96 \\sim O97 \\sim O98 \\sim O99 \\sim
O100 \\sim O101 \\sim O102 \\sim O103 \\sim O104 \\sim O105 \\sim O106 \\sim
O107 \\sim O108 \\sim O109 \\sim O110 \\sim O111 \\sim O112 \\sim O113 \\sim
O114 \\sim O115 \\sim O116 \\sim O115: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Sc1 \\sim O131 \\sim Nb40 \\sim O122 \\sim O167 \\sim O64 \\sim O62 \\sim O91:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
K1 \\sim K2 \\sim K3 \\sim K4 \\sim K4A \\sim K5 \\sim K6 \\sim K6A \\sim K7
\\sim K8 \\sim K9 \\sim K6B \\sim Na1 \\sim Na2 \\sim Na4 \\sim Na5 \\sim Na6
\\sim Na7 \\sim Na7A \\sim Na8B \\sim Na9 \\sim Na10 \\sim Na11 \\sim Na12
\\sim Na13 \\sim Na16 \\sim Na17 \\sim Na18 \\sim Na19 \\sim Na20 \\sim Na25
\\sim Na21 \\sim Na15 \\sim Na26 \\sim Na27 \\sim K10B \\sim K10A \\sim Na8A
\\sim O24A \\sim O24B \\sim O157: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Nb1 \\sim Nb2 \\sim Nb3 \\sim Nb4 \\sim Nb5 \\sim Nb6 \\sim Nb7: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Nb1A \\sim Nb2A \\sim Nb3A \\sim Nb4A \\sim Nb5A \\sim Nb6A \\sim Nb7A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O182) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(K1) \\sim Ueq, Uanis(K2) \\sim Ueq, Uanis(K3) \\sim Ueq, Uanis(K4) \\sim
Ueq, Uanis(K4A) \\sim Ueq, Uanis(K5) \\sim Ueq, Uanis(K6) \\sim Ueq, Uanis(K6A)
\\sim Ueq, Uanis(K7) \\sim Ueq, Uanis(K8) \\sim Ueq, Uanis(K9) \\sim Ueq,
Uanis(K6B) \\sim Ueq, Uanis(Na1) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(Na4)
\\sim Ueq, Uanis(Na5) \\sim Ueq, Uanis(Na6) \\sim Ueq, Uanis(Na7) \\sim Ueq,
Uanis(Na7A) \\sim Ueq, Uanis(Na8B) \\sim Ueq, Uanis(Na9) \\sim Ueq, Uanis(Na10)
\\sim Ueq, Uanis(Na11) \\sim Ueq, Uanis(Na12) \\sim Ueq, Uanis(Na13) \\sim Ueq,
Uanis(Na16) \\sim Ueq, Uanis(Na17) \\sim Ueq, Uanis(Na18) \\sim Ueq,
Uanis(Na19) \\sim Ueq, Uanis(Na20) \\sim Ueq, Uanis(Na25) \\sim Ueq,
Uanis(Na21) \\sim Ueq, Uanis(Na15) \\sim Ueq, Uanis(Na26) \\sim Ueq,
Uanis(Na27) \\sim Ueq, Uanis(K10B) \\sim Ueq, Uanis(K10A) \\sim Ueq,
Uanis(Na8A) \\sim Ueq, Uanis(O24A) \\sim Ueq, Uanis(O24B) \\sim Ueq,
Uanis(O157) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Nb1) \\sim Ueq, Uanis(Nb2) \\sim Ueq, Uanis(Nb3) \\sim Ueq, Uanis(Nb4)
\\sim Ueq, Uanis(Nb5) \\sim Ueq, Uanis(Nb6) \\sim Ueq, Uanis(Nb7) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Nb1A) \\sim Ueq, Uanis(Nb2A) \\sim Ueq, Uanis(Nb3A) \\sim Ueq,
Uanis(Nb4A) \\sim Ueq, Uanis(Nb5A) \\sim Ueq, Uanis(Nb6A) \\sim Ueq,
Uanis(Nb7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24A) \\sim Ueq, Uanis(O24B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O13W) \\sim Ueq, Uanis(O20B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O154) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O184) = Uanis(O157) = Uanis(O201)
3. Others
 Sof(K10B)=Sof(O154)=1-FVAR(1)
 Sof(K10A)=Sof(O1B)=FVAR(1)
 Fixed Sof: Na1(0.5) Na2(0.5) Na4(0.5) Na7(0.8) Na7A(0.2) Na8B(0.84) Na9(0.5)
 Na12(0.5) Na13(0.5) Na16(0.5) Na17(0.5) Na20(0.7) Na25(0.3) Na15(0.5)
 Na26(0.5) Na27(0.5) K4(0.75) K4A(0.25) K6(0.57) K6A(0.3) Nb1(0.5) Nb2(0.5)
 Nb3(0.5) Nb4(0.5) Nb5(0.5) Nb6(0.5) Nb7(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5)
 O5(0.5) O6(0.5) O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5) O12(0.5) O13(0.5)
 O14(0.5) O15(0.5) O16(0.5) O17(0.5) O18(0.5) O20(0.5) Nb1A(0.5) Nb2A(0.5)
 Nb3A(0.5) Nb4A(0.5) Nb5A(0.5) Nb6A(0.5) Nb7A(0.5) O1A(0.5) O2A(0.5) O3A(0.5)
 O4A(0.5) O5A(0.5) O6A(0.5) O7A(0.5) O8A(0.5) O9A(0.5) O10A(0.5) O11A(0.5)
 O12A(0.5) O13A(0.5) O14A(0.5) O15A(0.5) O16A(0.5) O17A(0.5) O18A(0.5)
 O20A(0.5) O20B(0.5) O20C(0.5) O24A(0.5) O24B(0.5) O157(0.5) O185(0.5)
 O200(0.5) O208(0.5) O6W(0.5) O12W(0.5) O201(0.5) O13W(0.5) O16W(0.5) O15W(0.3)
 K6B(0.13) Na8A(0.16) O15X(0.7)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1413 electrons were 
found in a volume of 3698\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
71[H2O] per Asymmetric Unit 
which account for 1420 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13200
_shelx_hkl_checksum              20784
_shelx_fab_checksum              12120
_olex2_submission_special_instructions 'No special instructions were received'