The anion-binding polyanion: a molecular cobalt vanadium oxide with anion-sensitive visual response
Andrey Seliverstov; Johannes Forster; Magdalena Heiland; Johannes Unfried; Carsten Streb; Chem.Commun. 50 (2014) 7840–; doi:10.1039/C4CC03827D

data_7115282
_publ_section_title
;
 The anion-binding polyanion: a molecular cobalt vanadium oxide with
 anion-sensitive visual response
;
_journal_name_full               Chem.Commun.
_journal_page_first              7840
_journal_paper_doi               10.1039/C4CC03827D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C7 H5 Co O14 V4, 3(C16 H36 N)'
_chemical_formula_sum            'C55 H113 Co N3 O14 V4'
_chemical_formula_weight         1303.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9267(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1500(4)
_cell_length_b                   23.6855(4)
_cell_length_c                   23.9678(4)
_cell_measurement_reflns_used    18163
_cell_measurement_temperature    180.00(14)
_cell_measurement_theta_max      30.2040
_cell_measurement_theta_min      3.2310
_cell_volume                     13677.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3385
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018426000
_diffrn_orient_matrix_UB_12      0.0249768000
_diffrn_orient_matrix_UB_13      -0.0163548000
_diffrn_orient_matrix_UB_21      -0.0293465000
_diffrn_orient_matrix_UB_22      -0.0024018000
_diffrn_orient_matrix_UB_23      -0.0022950000
_diffrn_orient_matrix_UB_31      -0.0015039000
_diffrn_orient_matrix_UB_32      0.0163386000
_diffrn_orient_matrix_UB_33      0.0246434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            54985
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.630
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.799
_diffrn_reflns_theta_min         3.080
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.2379
_exptl_crystal_size_mid          0.1958
_exptl_crystal_size_min          0.1528
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 6766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.018(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1414
_refine_ls_number_reflns         31955
_refine_ls_number_restraints     3829
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0431P)^2^+7.3122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.394
_reflns_Friedel_fraction_full    0.497
_reflns_Friedel_fraction_max     0.356
_reflns_number_gt                25362
_reflns_number_total             31955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03827d2.cif
_cod_data_source_block           as14031
_cod_database_code               7115282
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Co V4 O12 C7 H5 O2'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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
 C99-C76
 1.52 with sigma of 0.02
 C110-C109 = C109-C99 = C99-C76
 1.52 with sigma of 0.02
 C99-C109 = C112-C109 = C112-C76 = C99-C76 = C111-C109 = C110-C109
 1.52 with sigma of 0.02
 C99-C113 = C111-C113 = C99-C76 = C112-C76 = C110-C109 = C112-C109
 1.54 with sigma of 0.02
 C99-C76 \\sim C26-C1 \\sim C26-C21 \\sim C4-C35 \\sim C9-C6 \\sim C55-C19
\\sim C72-C21 \\sim C56-C35 ~
 C9-C3 \\sim C55-C24 \\sim C87-C56 \\sim C3-C18 \\sim C40-C24 \\sim C69-C12
\\sim C54-C13 \\sim C31-C22 ~
 C70-C23 \\sim C80-C69 \\sim C54-C15 \\sim C73-C31 \\sim C70-C66 \\sim C84-C80
\\sim C38-C15 \\sim C73-C105
 \\sim C66-C107 \\sim C28-C10 \\sim C59-C25 \\sim C39-C32 \\sim C63-C62 \\sim
C50-C28 \\sim C59-C51 \\sim C39-
 C36 \\sim C74-C63 \\sim C90-C50 \\sim C98-C51 \\sim C97-C36 \\sim C82-C74
\\sim C47-C2 \\sim C47-C41 \\sim C5-
 C20 \\sim C33-C27 \\sim C58-C53 \\sim C77-C41 \\sim C29-C20 \\sim C52-C33
\\sim C58-C37 \\sim C78-C29 ~
 C52-C48 \\sim C37-C101 \\sim C16-C11 \\sim C86-C14 \\sim C57-C42 \\sim C49-C46
\\sim C34-C16 \\sim C88-C86
 \\sim C83-C57 \\sim C81-C49 \\sim C45-C34 \\sim C88-C103 \\sim C85-C83 \\sim
C81-C102 \\sim C71-C61 \\sim C75-
 C71 \\sim C79-C64 \\sim C67-C104 \\sim C89-C75 \\sim C79-C100 \\sim C106-C104
\\sim C99-C109 \\sim C108-
 C100 \\sim C95-C106 \\sim C110-C109
 with sigma of 0.02
 N4-C2 \\sim N2-C1 \\sim N2-C4 \\sim N2-C6 \\sim N2-C19 \\sim N1-C12 \\sim
N1-C13 \\sim N1-C22 \\sim N1-C23 ~
 N3-C10 \\sim N3-C25 \\sim N3-C32 \\sim N3-C62 \\sim N4-C5 \\sim N4-C27 \\sim
N4-C53 \\sim N5-C11 \\sim N5-C14
 \\sim N5-C42 \\sim N5-C46 \\sim N6-C61 \\sim N6-C64 \\sim N6-C67 \\sim N6-C76
 with sigma of 0.02
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79,
 C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95,
  C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108, N1,
 N2, N3, N4, N5, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99, C109, C110
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C110, C109, C99
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48,
 C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63, C64,
  C65, C66, C67, C68, C69, C70, C71, C72, C73, C74, C75, C76, C77, C78, C79,
 C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90, C91, C92, C93, C94, C95,
  C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108,
 C109, C110, N1, N2, N3, N4, N5, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C111, C110, C109, C99, C112, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim N1 \\sim N2 \\sim N3 \\sim N4
\\sim N5 \\sim N6: within 1.7A with sigma of 0.04 and sigma for terminal atoms
of 0.08
C99: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C110 \\sim C109 \\sim C99: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C112 \\sim C99 \\sim C76 \\sim C109 \\sim C111 \\sim C110: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C99) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C99) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C111) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C99) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C95) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H76c(0.5) H76d(0.5) H76a(0.5) H76b(0.5) C99(0.5) H99a(0.5)
 H99b(0.5) C109(0.5) H10j(0.5) H10k(0.5) C110(0.5) H11a(0.5) H11b(0.5)
 H11c(0.5) C111(0.5) H11d(0.5) H11e(0.5) H11f(0.5) C112(0.5) H11g(0.5)
 H11h(0.5) C113(0.5) H11i(0.5) H11j(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C9(H9a,H9b), C10(H10r,H10s), C11(H11k,H11l), C12(H12a,H12b), C13(H13a,H13b),
 C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C19(H19a,H19b), C20(H20a,H20b),
  C21(H21a,H21b), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,
 H25b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b),
 C31(H31a,H31b), C32(H32a,H32b), C33(H33a,H33b), C34(H34a,H34b), C35(H35a,H35b),
  C36(H36a,H36b), C37(H37a,H37b), C39(H39a,H39b), C41(H41a,H41b), C42(H42a,
 H42b), C46(H46a,H46b), C47(H47a,H47b), C49(H49a,H49b), C50(H50a,H50b),
 C51(H51a,H51b), C52(H52a,H52b), C53(H53a,H53b), C54(H54a,H54b), C55(H55a,H55b),
  C56(H56a,H56b), C57(H57a,H57b), C58(H58a,H58b), C59(H59a,H59b), C61(H61a,
 H61b), C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b), C66(H66a,H66b),
 C67(H67a,H67b), C69(H69a,H69b), C70(H70a,H70b), C71(H71a,H71b), C73(H73a,H73b),
  C74(H74a,H74b), C75(H75a,H75b), C76(H76c,H76d), C76(H76a,H76b), C79(H79a,
 H79b), C80(H80a,H80b), C81(H81a,H81b), C83(H83a,H83b), C86(H86a,H86b),
 C88(H88a,H88b), C99(H99a,H99b), C100(H10a,H10b), C104(H10c,H10d), C106(H10e,
 H10f), C109(H10j,H10k), C112(H11g,H11h), C113(H11i,H11j)
6.b Me refined with riding coordinates:
 C18(H18a,H18b,H18c), C38(H38a,H38b,H38c), C40(H40a,H40b,H40c), C45(H45a,H45b,
 H45c), C48(H48a,H48b,H48c), C72(H72a,H72b,H72c), C77(H77a,H77b,H77c), C78(H78a,
 H78b,H78c), C82(H82a,H82b,H82c), C84(H84a,H84b,H84c), C85(H85a,H85b,H85c),
 C87(H87a,H87b,H87c), C89(H89a,H89b,H89c), C90(H90a,H90b,H90c), C95(H95a,H95b,
 H95c), C97(H97a,H97b,H97c), C98(H98a,H98b,H98c), C101(H10t,H10u,H10v),
 C102(H10w,H10x,H10y), C103(H10z,H,Ha), C105(H10l,H10m,H10n), C107(H10o,H10p,
 H10q), C108(H10g,H10h,H10i), C110(H11a,H11b,H11c), C111(H11d,H11e,H11f)
6.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C60(H60), C65(H65), C68(H68), C91(H91), C92(H92),
 C93(H93), C94(H94), C96(H96)
;
_shelx_res_checksum              46756
_ins_header
;
TITL AS14031 in Cc 
REM Cc (#9 in standard setting)
CELL 0.71073  24.150027  23.685466  23.967799  90.0000  93.9267  90.0000
ZERR   30.00   0.000370   0.000370   0.000350   0.0000   0.0014   0.0000
LATT -7
SYMM  x,-y, z+1/2 
SFAC C H O V Co
UNIT 210.00 150.00 420.00 120.00 30.00
TREF
HKLF 4
END
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'