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_7042541
_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         'C30 H50 O23 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C62 H122 N2 O23 V6'
_chemical_formula_weight         1569.25
_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                78.38(3)
_cell_angle_beta                 89.80(3)
_cell_angle_gamma                62.09(3)
_cell_formula_units_Z            1
_cell_length_a                   11.562(2)
_cell_length_b                   12.318(3)
_cell_length_c                   15.050(3)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      31.4970
_cell_measurement_theta_min      2.3161
_cell_volume                     1845.1(9)
_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      173.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18958
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       Prism
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7224
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0576P)^2^+1.9644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6754
_reflns_number_total             7224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           kuixi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7042538--7042542.cif.
;
_cod_original_cell_volume        1845.0(8)
_cod_database_code               7042541
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C20, O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C20 \\sim O17: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C11(H11A,H11B), C26(H26A,H26B), C16(H16A,H16B),
 C19(H19A,H19B), C1(H1A,H1B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B),
  C1A(H1AA,H1AB), C1C(H1CA,H1CB)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23)
4.c X=CH2 refined with riding coordinates:
 C25(H25A,H25B)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C1B(H1BA,H1BB,H1BC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,
 H1EC)
;
_shelx_res_checksum              64151
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'