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_7042539
_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         'C24 H42 O29 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C56 H114 N2 O29 V6'
_chemical_formula_weight         1585.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-10
_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                 108.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.504(3)
_cell_length_b                   17.740(4)
_cell_length_c                   15.324(3)
_cell_measurement_reflns_used    12190
_cell_measurement_temperature    153.1500
_cell_measurement_theta_max      29.1270
_cell_measurement_theta_min      1.9624
_cell_volume                     3478.5(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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      153.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0683P)^2^+3.6987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6264
_reflns_number_total             6820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           qinshui
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_original_cell_volume        3478.5(13)
_cod_database_code               7042539
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C1E-C1D
 1.4 with sigma of 0.001
3. Rigid bond restraints
 C1F, C1H, C1I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1F \\sim C1H \\sim C1I: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002
5. Others
 Sof(H1FC)=Sof(H1FD)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=1-FVAR(1)
 Sof(H1FA)=Sof(H1FB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C7(H7A,H7B), C1(H1A,H1B), C2(H2A,
 H2B), C15(H15A,H15B), C17(H17A,H17B), C20(H20A,H20B), C3(H3A,H3B), C4(H4A,H4B),
  C5(H5A,H5B), C6(H6A,H6B), C10(H10A,H10B), C13(H13A,H13B), C16(H16A,H16B),
 C19(H19A,H19B), C1A(H1AA,H1AB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1F(H1FC,H1FD),
  C1G(H1GA,H1GB)
6.b Me refined with riding coordinates:
 C1D(H1DA,H1DB,H1DC), C1I(H1IA,H1IB,H1IC)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1H(H1HA,H1HB,
 H1HC)
;
_shelx_res_checksum              6408
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'