A new family of anionic organic-inorganic hybrid doughnut-like nanostructures
Zhuxiu Zhang; Wen-Yang Gao; Lukasz Wojtas; Zhenjie Zhang; Michael J. Zaworotko; Chem.Commun. 51 (2015) 9223–; doi:10.1039/C5cc02719E

data_7117197
_publ_section_title
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 A new family of anionic organic-inorganic hybrid doughnut-like
 nanostructures
;
_journal_name_full               Chem.Commun.
_journal_page_first              9223
_journal_paper_doi               10.1039/C5cc02719E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'C64 H32 O64 V16, 4(Cl), 3(C2 H8 N), 6(C3 H7 N O), 9(O2.5), 2(C H4 N0.5 O0.13)'
_chemical_formula_sum            'C90 H106 Cl4 N10 O92.75 V16'
_chemical_formula_weight         3768.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.8678(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.2958(6)
_cell_length_b                   21.3300(6)
_cell_length_c                   21.9581(6)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.04
_cell_measurement_theta_min      2.99
_cell_volume                     9594.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83383
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.668
_diffrn_reflns_theta_max         66.668
_diffrn_reflns_theta_min         2.944
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.485
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1346 before and 0.0861 after correction.
The Ratio of minimum to maximum transmission is 0.6460.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       plate
_exptl_crystal_F_000             3788
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         16852
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1555P)^2^+24.5321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2886
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9906
_reflns_number_total             16852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02719e2.cif
_cod_data_source_block           DMA_hydoughnut-1
_cod_database_code               7117197
_shelx_estimated_absorpt_t_max   0.586
_shelx_estimated_absorpt_t_min   0.522
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C42
 1.31 with sigma of 0.02
 N3_$1-C38_$1
 1.31 with sigma of 0.02
 N2-C35
 1.31 with sigma of 0.02
 N5-C45
 1.31 with sigma of 0.02
 N6B-C1C
 1.31 with sigma of 0.02
 N6A-C47A = N6A-C48A
 1.47 with sigma of 0.02
 N7BB-C1A
 1.47 with sigma of 0.01
 N0AA-C4AA
 1.31 with sigma of 0.02
 N8-C76
 1.32 with sigma of 0.02
 O33-C35
 1.24 with sigma of 0.02
 O38-C45
 1.24 with sigma of 0.02
 O9AA-C1C
 1.24 with sigma of 0.02
 O85-C4AA
 1.24 with sigma of 0.02
 O77-C76
 1.23 with sigma of 0.02
 N8-O77
 2.26 with sigma of 0.02
 O35-C42
 1.24 with sigma of 0.02
 N2-C37 = N2-C36
 1.47 with sigma of 0.02
 H36A-H37A
 -2.2 with sigma of 0.02
 N4-C41 = N4-C43
 1.45 with sigma of 0.02
 H41A-H43A
 -2.2 with sigma of 0.02
 N8-C77 = N8-C78
 1.45 with sigma of 0.02
 C77-C78
 2.47 with sigma of 0.02
 C78-C76
 2.41 with sigma of 0.02
 C76-C77
 2.41 with sigma of 0.02
 H77A-H78A
 -2.2 with sigma of 0.02
 N6B-C47B = N6B-C48B
 1.47 with sigma of 0.02
 H48A-H47A
 -2.2 with sigma of 0.02
 H47C-H19
 -2.2 with sigma of 0.02
 N5-C44 = N5-C46
 1.45 with sigma of 0.02
 H46A-H44A
 -2.2 with sigma of 0.02
 N3_$1-C39_$1 = N3_$1-C40_$1
 1.45 with sigma of 0.02
 H40B-H39B
 -2.2 with sigma of 0.02
 N7BB-C1A = N7BB-C1D = N0AA-C3 = N0AA-C6
 1.47 with sigma of 0.01
 H3A-H6A
 -2.2 with sigma of 0.02
 C47A-C48A
 2.47 with sigma of 0.04
 C1A-C1D
 2.47 with sigma of 0.04
 O33-N2
 2.26 with sigma of 0.04
 O38-N5
 2.26 with sigma of 0.04
 N6B-O9AA
 2.26 with sigma of 0.04
 N0AA-O85
 2.26 with sigma of 0.04
 O35-N4
 2.26 with sigma of 0.04
 O34-N3
 2.26 with sigma of 0.04
 C36-C37
 2.47 with sigma of 0.04
 C35-C37
 2.41 with sigma of 0.04
 C35-C36
 2.41 with sigma of 0.04
 C42-C41
 2.41 with sigma of 0.04
 C41-C43
 2.47 with sigma of 0.04
 C43-C42
 2.41 with sigma of 0.04
 C48B-C47B
 2.47 with sigma of 0.04
 C1C-C47B
 2.41 with sigma of 0.04
 C1C-C48B
 2.41 with sigma of 0.04
 C47B-C48B
 2.5 with sigma of 0.04
 C46-C44
 2.47 with sigma of 0.04
 C46-C45
 2.41 with sigma of 0.04
 C45-C44
 2.41 with sigma of 0.04
 C40-C38
 2.41 with sigma of 0.04
 C38-C39
 2.41 with sigma of 0.04
 C39-C40
 2.47 with sigma of 0.04
 C3-C4AA
 2.41 with sigma of 0.04
 C4AA-C6
 2.41 with sigma of 0.04
 C3-C6
 2.5 with sigma of 0.04
3. Restrained planarity
 C36, C37, N2, C35, O33
 with sigma of 0.1
 C41, N4, C42, C43, O35
 with sigma of 0.1
 O77, C76, N8, C77, C78
 with sigma of 0.1
 O9AA, C1C, N6B, C48B, C47B
 with sigma of 0.1
 O38, C45, N5, C44, C46
 with sigma of 0.1
 C39, N3, C38, O34, C40
 with sigma of 0.1
 O85, C4AA, N0AA, C3, C6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N2 \\sim C35: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1C \\sim N6B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C47A \\sim N6A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C48A \\sim N6A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N0AA \\sim C4AA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1C \\sim O9AA: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O85: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C43 \\sim N4 \\sim C42 \\sim O35 \\sim C41: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
N0AA \\sim C6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(N4)=Sof(O35)=Sof(C42)=Sof(H42)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(1)
 Sof(O34)=Sof(N3)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1BC(0.25) H1BD(0.25) H1CE(0.25) H1CF(0.25)
 C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5) O33(0.5) C37(0.5)
 H37A(0.5) H37B(0.5) H37C(0.5) N2(0.5) O36(0.5) O37(0.5) C44(0.5) H44A(0.5)
 H44B(0.5) H44C(0.5) O38(0.5) N5(0.5) C45(0.5) H45(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C47B(0.5) H47A(0.5) H47B(0.5) H47C(0.5) N6B(0.5) C48B(0.5)
 H48A(0.5) H48B(0.5) H48C(0.5) N7BB(0.5) H7BA(0.5) H7BB(0.5) C1A(0.5) H1AC(0.5)
 H1AD(0.5) H1AE(0.5) O39(0.5) C21(0.25) H21A(0.25) H21B(0.25) H21C(0.25)
 C33(0.25) H33A(0.25) H33B(0.25) H33C(0.25) O42(0.5) O43(0.5) O41(0.25)
 O44(0.25) O48(0.25) C78(0.25) H78A(0.25) H78B(0.25) H78C(0.25) O12(0.25)
 O16(0.25) O47(0.25) O54(0.25) O7AA(0.25) O3(0.25) O55(0.25) O53(0.5) N8(0.25)
 C52(0.25) H52A(0.25) H52B(0.25) H52C(0.25) O51(0.25) O49(0.125) O56(0.25)
 O13(0.25) O19(0.25) O58(0.25) O59(0.25) O57(0.25) O60(0.25) O9AA(0.5)
 O61(0.25) O63(0.5) O64(0.25) O65(0.125) O66(0.125) O67(0.25) O70(0.125)
 O69(0.125) O68(0.25) O71(0.125) C74(0.25) H74A(0.25) H74B(0.25) H74C(0.25)
 C77(0.25) H77A(0.25) H77B(0.25) H77C(0.25) O79(0.125) O83(0.125) O81(0.125)
 O84(0.125) O11(0.125) O77(0.25) O80(0.125) O82(0.25) O20(0.125) O85(0.25)
 C76(0.25) H76(0.25) O2(0.125) O5(0.125) O88(0.125) O89(0.125) C1C(0.5)
 H1C(0.5) N6A(0.5) H6AA(0.5) H6AB(0.5) C47A(0.5) H47D(0.5) H47E(0.5) H47F(0.5)
 C48A(0.5) H48D(0.5) H48E(0.5) H48F(0.5) C1D(0.5) H1DA(0.5) H1DB(0.5) H1DC(0.5)
 N0AA(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C6(0.25) H6A(0.25) H6B(0.25)
 H6C(0.25) C4AA(0.25) H4AA(0.25)
6.a Riding coordinates:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C78(H78A,H78B,H78C), C77(H77A,H77B,H77C), C3(H3A,H3B,H3C), C6(H6A,H6B,
 H6C)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1AA,H1AB), N1(H1BC,H1BD), N1(H1CE,H1CF), N7BB(H7BA,H7BB), N6A(H6AA,H6AB)
6.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C1A(H1AC,H1AD,H1AE), C21(H21A,H21B,
 H21C), C33(H33A,H33B,H33C), C52(H52A,H52B,H52C), C74(H74A,H74B,H74C),
 C47A(H47D,H47E,H47F), C48A(H48D,H48E,H48F), C1D(H1DA,H1DB,H1DC)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C16(H16), C17(H17), C19(H19), C20(H20), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
  C35(H35), C38(H38), C42(H42), C45(H45), C76(H76), C1C(H1C), C4AA(H4AA)
6.e Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C47B(H47A,H47B,H47C), C48B(H48A,H48B,H48C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'