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_7042540
_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         '2(C7 H8 F3 O11.5 V3), 2(C16 H36 N)'
_chemical_formula_sum            'C46 H88 F6 N2 O23 V6'
_chemical_formula_weight         1456.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 102.9704(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5215(4)
_cell_length_b                   15.8480(2)
_cell_length_c                   18.2434(3)
_cell_measurement_reflns_used    11294
_cell_measurement_temperature    105.5
_cell_measurement_theta_max      29.1806
_cell_measurement_theta_min      3.0412
_cell_volume                     6345.32(18)
_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
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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
;
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      105.5
_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    9.00   35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609   77.0000 -120.0000 26

  2 omega  -46.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609   77.0000   90.0000 35

  3 omega  -86.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0609  -77.0000  -90.0000 98

  4 omega   10.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -53.0000  -65.0000 26

  5 omega   20.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000  -60.0000 26

  6 omega  -38.00   18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   30.0000 56

  7 omega   -5.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   37.0000 -150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0034430000
_diffrn_orient_matrix_UB_12      -0.0286628000
_diffrn_orient_matrix_UB_13      0.0286251000
_diffrn_orient_matrix_UB_21      0.0321217000
_diffrn_orient_matrix_UB_22      -0.0033836000
_diffrn_orient_matrix_UB_23      0.0118683000
_diffrn_orient_matrix_UB_31      0.0002784000
_diffrn_orient_matrix_UB_32      0.0342248000
_diffrn_orient_matrix_UB_33      0.0251405000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39135
_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         3.047
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.727
_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    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.656
_refine_diff_density_min         -1.587
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         12449
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+12.8423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1071
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10379
_reflns_number_total             12449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00274b2.cif
_cod_data_source_block           exp_sanfuyichun
_cod_depositor_comments
'Adding full bibliography for 7042538--7042542.cif.'
_cod_original_cell_volume        6345.29(19)
_cod_database_code               7042540
_reflns_odcompleteness_completeness 99.72
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C7, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C7 \\sim C12 \\sim C13: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C11 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) = Uanis(C1A)
Uanis(C15) = Uanis(C8) = Uanis(C1D)
Uanis(C1C) = Uanis(C1E)
Uanis(N) = Uanis(C1) = Uanis(C10)
Uanis(C42) = Uanis(O25) = Uanis(O55)
4. Others
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(H1AF)=1-FVAR(2)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C18)=Sof(H18A)=
 Sof(H18B)=Sof(H18C)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=FVAR(2)
 Sof(H3BC)=Sof(H3BD)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C1E)=Sof(H1EA)=
 Sof(H1EB)=1-FVAR(3)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=FVAR(3)
 Sof(H65C)=Sof(H65D)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=1-FVAR(4)
 Sof(H65A)=Sof(H65B)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C35(H35A,H35B), C38(H38A,H38B), C41(H41A,H41B), C43(H43A,
 H43B), C50(H50A,H50B), C56(H56A,H56B), C61(H61A,H61B), C65(H65A,H65B),
 C65(H65C,H65D), C77(H77A,H77B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C39(H39A,H39B), C40(H40A,H40B), C44(H44A,
 H44B), C46(H46A,H46B), C52(H52A,H52B), C53(H53A,H53B), C57(H57A,H57B), C1(H1A,
 H1B), C3(H3AA,H3AB), C3(H3BC,H3BD), C5(H5A,H5B), C7(H7A,H7B), C0AA(H0AA,H0AB),
 C11(H11A,H11B), C12(H12A,H12B), C10(H10A,H10B), C21(H21A,H21B), C2(H2A,H2B),
 C9(H9A,H9B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B),
 C1B(H1BA,H1BB), C8(H8A,H8B), C15(H15A,H15B), C1E(H1EA,H1EB)
5.b Me refined with riding coordinates:
 C1A(H1AD,H1AE,H1AF)
5.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C59(H59A,H59B,H59C), C64(H64A,H64B,H64C), C67(H67A,H67B,
 H67C), C4(H4A,H4B,H4C), C1AA(H1AA,H1AB,H1AC), C13(H13A,H13B,H13C), C6(H6A,H6B,
 H6C), C1C(H1CA,H1CB,H1CC), C18(H18A,H18B,H18C), C1D(H1DA,H1DB,H1DC)
;
_shelx_res_checksum              10549
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'