A simple synthetic route to polyoxovanadate-based organic-inorganic hybrids using EEDQ as an ester coupling agent.
Bayaguud, Aruuhan; Li, JianDa; She, Shan; Wei, Yongge; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4602–4608; doi:10.1039/c7dt00274b

data_7042542
_publ_section_title
;
 A simple synthetic route to polyoxovanadate-based organic-inorganic
 hybrids using EEDQ as an ester coupling agent.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4602
_journal_page_last               4608
_journal_paper_doi               10.1039/c7dt00274b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C42 H78 O23 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C74 H150 N2 O23 V6'
_chemical_formula_weight         1741.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-10 deposited with the CCDC.
2017-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.329(4)
_cell_angle_beta                 96.637(5)
_cell_angle_gamma                116.297(5)
_cell_formula_units_Z            1
_cell_length_a                   11.4081(7)
_cell_length_b                   11.9363(6)
_cell_length_c                   18.8822(11)
_cell_measurement_reflns_used    5270
_cell_measurement_temperature    105.6
_cell_measurement_theta_max      29.1498
_cell_measurement_theta_min      2.9927
_cell_volume                     2199.3(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      105.6
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -36.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -77.0000 -150.0000 33

  2 omega   29.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -84.0000  139.0000 25

  3 omega   -9.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000  -60.0000 93

  4 omega    7.00   39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000   30.0000 32

  5 omega  -45.00   45.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   30.0000 90

  6 omega   -5.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   37.0000 -150.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0238049000
_diffrn_orient_matrix_UB_12      -0.0064105000
_diffrn_orient_matrix_UB_13      0.0328334000
_diffrn_orient_matrix_UB_21      0.0464902000
_diffrn_orient_matrix_UB_22      -0.0209505000
_diffrn_orient_matrix_UB_23      0.0114880000
_diffrn_orient_matrix_UB_31      0.0484932000
_diffrn_orient_matrix_UB_32      0.0654348000
_diffrn_orient_matrix_UB_33      0.0184407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15055
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       'flat stick'
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0206P)^2^+0.9031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7165
_reflns_number_total             8630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           exp_shiliuchun
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_original_cell_volume        2199.3(2)
_cod_database_code               7042542
_shelx_estimated_absorpt_t_max   0.948
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_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C22(H22A,H22B), C32(H32A,H32B), C30(H30A,H30B), C34(H34A,
 H34B), C2(H2A,H2B), C24(H24A,H24B), C35(H35A,H35B), C31(H31A,H31B), C1(H1A,
 H1B), C3(H3A,H3B), C23(H23A,H23B), C28(H28A,H28B), C27(H27A,H27B), C6(H6A,H6B),
  C36(H36A,H36B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B),
 C19(H19A,H19B), C15(H15A,H15B), C16(H16A,H16B), C8(H8A,H8B), C17(H17A,H17B),
 C20(H20A,H20B), C12(H12A,H12B), C14(H14A,H14B), C11(H11A,H11B), C18(H18A,H18B)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              44450
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'