Versatile post-functionalisation strategy for the formation of modular organic-inorganic polyoxometalate hybrids.
Salazar Marcano, David E.; Moussawi, Mhamad Aly; Anyushin, Alexander V.; Lentink, Sarah; Van Meervelt, Luc; Ivanović-Burmazović, Ivana; Parac-Vogt, Tatjana N; Chemical science 13 (2022) 2891–2899; doi:10.1039/d1sc06326j

data_1566333
_publ_section_title
;
 Versatile post-functionalisation strategy for the formation of modular
 organic-inorganic polyoxometalate hybrids.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              2891
_journal_page_last               2899
_journal_paper_doi               10.1039/d1sc06326j
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C10 H19 O13.5 V3, C16 H36 N'
_chemical_formula_sum            'C26 H55 N O13.5 V3'
_chemical_formula_weight         750.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-06 deposited with the CCDC.	2022-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.803(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0520(12)
_cell_length_b                   13.4949(9)
_cell_length_c                   20.5929(10)
_cell_measurement_reflns_used    6373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.9150
_cell_measurement_theta_min      2.8970
_cell_volume                     3506.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9631
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -93.00 -35.00   1.00   30.00    --  -17.07-178.00 -90.00   58
  2  \w    -90.00  56.00   1.00   30.00    --  -17.07   0.00 150.00  146
  3  \w     34.00  95.00   1.00   30.00    --   18.87-178.00   0.00   61
  4  \w    -87.00  13.00   1.00   30.00    --  -17.07 -77.00  90.00  100
  5  \w    -20.00  25.00   1.00   30.00    --  -17.07 -99.00 -60.00   45
  6  \w    -43.00  55.00   1.00   30.00    --  -17.07  38.00-150.00   98
  7  \w    -20.00  13.00   1.00   30.00    --   18.87 -99.00  90.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0463760000
_diffrn_orient_matrix_UB_12      -0.0103474000
_diffrn_orient_matrix_UB_13      -0.0257816000
_diffrn_orient_matrix_UB_21      -0.0228187000
_diffrn_orient_matrix_UB_22      0.0451344000
_diffrn_orient_matrix_UB_23      0.0070347000
_diffrn_orient_matrix_UB_31      0.0221896000
_diffrn_orient_matrix_UB_32      0.0248215000
_diffrn_orient_matrix_UB_33      -0.0235505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            38832
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.542
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+8.4208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2097
_refine_ls_wR_factor_ref         0.2460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3732
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06326j2.cif
_cod_data_source_block           tpv2008_tw
_cod_depositor_comments
'Adding full bibliography for 1566332--1566333.cif.'
_cod_original_cell_volume        3506.8(4)
_cod_original_formula_sum        'C26 H55 N O13.50 V3'
_cod_database_code               1566333
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C52H110N2O27V6
_chemical_oxdiff_usercomment     AA0070-MeOH+AcN/Et2O
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.786
_diffrn_oxdiff_ac4_digest_frames
;
011a00f3b689db7b124c9d8401d335b91f000273ff1
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.766(4)
 0.234(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 N28-C29 = N28-C33 = N28-C37 = N28-C41
 1.521 with sigma of 0.02
 C29-C30 = C33-C34 = C37-C38 = C41-C42
 1.511 with sigma of 0.02
 C30-C31 = C34-C35 = C38-C39 = C42-C43A = C42-C43B
 1.525 with sigma of 0.02
 C31-C32 = C35-C36 = C39-C40A = C39-C40B = C43A-C44A = C43B-C44B
 1.487 with sigma of 0.02
 N28-C30 = N28-C34 = N28-C38 = N28-C42
 2.568 with sigma of 0.04
 C29-C31 = C33-C35 = C37-C39 = C41-C43A = C41-C43B
 2.497 with sigma of 0.04
 C30-C32 = C34-C36 = C38-C40A = C38-C40B = C42-C44A = C42-C44B
 2.503 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C40A) = Uanis(C40B)
Uanis(C43A) = Uanis(C43B)
Uanis(C44A) = Uanis(C44B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=1-FVAR(2)
 Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C20(H20A,
 H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C39(H39C,H39D), C41(H41A,
 H41B), C42(H42A,H42B), C42(H42C,H42D), C43A(H43A,H43B), C43B(H43C,H43D)
7.b Me refined with riding coordinates:
 C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F)
7.c Tetrahedral OH refined with riding coordinates:
 O25(H25)
7.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40A(H40A,H40B,H40C), C40B(H40D,
 H40E,H40F)
7.e Idealised tetrahedral OH refined as rotating group:
 O23(H23), O27(H27)
;
_olex2_submission_original_sample_id 'AA0070 MeOH + ACN/Et2O'
_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 4.191
_oxdiff_exptl_absorpt_empirical_full_min 0.489