Post-functionalization through covalent modification of organic counter ions: a stepwise and controlled approach for novel hybrid polyoxometalate materials.
Kar, Aranya; Pradeep, Chullikkattil P.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12174–12179; doi:10.1039/d0dt01410a

data_7705294
_publ_section_title
;
 Post-functionalization through covalent modification of organic counter
 ions: a stepwise and controlled approach for novel hybrid polyoxometalate
 materials.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12174
_journal_page_last               12179
_journal_paper_doi               10.1039/d0dt01410a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'O40 Si W12, 4(C9 H11 O S), 2(C3 H7 N O)'
_chemical_formula_sum            'C42 H58 N2 O46 S4 Si W12'
_chemical_formula_weight         3689.43
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-06
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2020-01-12 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                92.730(4)
_cell_angle_beta                 101.278(5)
_cell_angle_gamma                104.065(5)
_cell_formula_units_Z            2
_cell_length_a                   13.3509(8)
_cell_length_b                   14.4698(7)
_cell_length_c                   19.8148(11)
_cell_measurement_reflns_used    6568
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.1270
_cell_measurement_theta_min      1.8790
_cell_volume                     3623.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9840
_diffrn_measured_fraction_theta_max 0.8465
_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    -52.00  66.00   1.00   38.18    --   26.84 -77.00  90.00  118
  2  \w    -53.00  66.00   1.00   38.18    --   26.84 -77.00-150.00  119
  3  \w    -52.00  67.00   1.00   38.18    --   26.84 -77.00 -30.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0528140000
_diffrn_orient_matrix_UB_12      -0.0243992000
_diffrn_orient_matrix_UB_13      -0.0158083000
_diffrn_orient_matrix_UB_21      -0.0176030000
_diffrn_orient_matrix_UB_22      0.0171508000
_diffrn_orient_matrix_UB_23      0.0289119000
_diffrn_orient_matrix_UB_31      -0.0060617000
_diffrn_orient_matrix_UB_32      0.0411784000
_diffrn_orient_matrix_UB_33      -0.0166279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19311
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.193
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             2764.000
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.068
_refine_diff_density_max         4.017
_refine_diff_density_min         -4.125
_refine_diff_density_rms         0.403
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         14724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+21.3553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                10869
_reflns_number_total             14724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt01410a2.cif
_cod_data_source_block           ak_47a_lt_cu
_cod_depositor_comments
'Adding full bibliography for 7705294--7705295.cif.'
_cod_original_cell_volume        3623.2(3)
_cod_database_code               7705294
_chemical_oxdiff_formula         'C84 H118 Mo24 N4 O92 S8 Si2 '
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C28(H28), C29(H29), C16(H16), C20(H20), C26(H26), C2(H2),
 C32(H32), C36(H36), C37(H37), C39(H39), C3(H3), C5(H5), C22(H22), C6(H6),
 C7(H7), C8(H8), C11(H11), C12(H12), C1D(H1D), C1G(H1G)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C40(H40A,H40B,
 H40C), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C1A(H1AA,
 H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1F(H1FA,H1FB,H1FC),
 C1E(H1EA,H1EB,H1EC)
;
_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 1.736
_oxdiff_exptl_absorpt_empirical_full_min 0.773