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_7042538
_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         'C34 H62 O25 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C66 H134 N2 O25 V6'
_chemical_formula_weight         1661.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-20
_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                90
_cell_angle_beta                 99.021(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2750(6)
_cell_length_b                   17.3035(7)
_cell_length_c                   27.3203(11)
_cell_measurement_reflns_used    4756
_cell_measurement_temperature    104.3
_cell_measurement_theta_max      29.3110
_cell_measurement_theta_min      3.2554
_cell_volume                     8532.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
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      104.3
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            19521
_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         25.999
_diffrn_reflns_theta_min         3.262
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.778
_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    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.006
_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     475
_refine_ls_number_reflns         8381
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0843
_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^)+(0.0647P)^2^+80.2263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5737
_reflns_number_total             8381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           exp_shiererchun
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_database_code               7042538
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.768
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H20 of O20, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H14 of O14
2. Restrained distances
 C16-C15
 1.53 with sigma of 0.02
 C17-C16
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C20, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, O20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C20 \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C15 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C17 \\sim O20: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(H17C)=Sof(H17D)=Sof(O20)=Sof(H20)=1-FVAR(1)
 Sof(O14)=Sof(H14)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(2)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
6.a Rotating group:
 O20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C30(H30A,H30B), C1(H1A,H1B), C27(H27A,H27B), C22(H22A,H22B),
 C3(H3A,H3B), C24(H24A,H24B), C23(H23A,H23B), C26(H26A,H26B), C20(H20A,H20B),
 C20(H20C,H20D), C18(H18A,H18B), C19(H19A,H19B), C32(H32A,H32B), C6(H6A,H6B),
 C28(H28A,H28B), C31(H31A,H31B), C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B),
 C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B), C11(H11A,H11B), C13(H13A,H13B),
 C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B), C17(H17C,H17D)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C33(H33A,H33B,
 H33C), C0AA(H0AA,H0AB,H0AC)
6.d Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_shelx_res_checksum              16328
_shelx_fab_checksum              1633
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'