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_7117200
_publ_section_title
;
 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
'C72 H48 Cl2 O72 V16, 5(Cl), 8(C2 H8 N), C3 H7 N O, 13.67(O0.75)'
_chemical_formula_sum            'C91 H119 Cl7 N9 O83.25 V16'
_chemical_formula_weight         3734.13
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-31 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                79.476(2)
_cell_angle_beta                 82.828(3)
_cell_angle_gamma                81.284(2)
_cell_formula_units_Z            1
_cell_length_a                   14.9214(6)
_cell_length_b                   16.0334(7)
_cell_length_c                   16.7794(7)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.871
_cell_measurement_theta_min      3.011
_cell_volume                     3881.7(3)
_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)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_laue_measured_fraction_full 0.927
_diffrn_reflns_laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47498
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.083
_diffrn_reflns_theta_min         2.828
_exptl_absorpt_coefficient_mu    9.656
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1117 before and 0.0738 after correction. The Ratio of minimum to maximum transmission is 0.6923. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       block
_exptl_crystal_F_000             1881
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         13009
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0755
_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^)+(0.0790P)^2^+24.4560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9331
_reflns_number_total             13009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02719e2.cif
_cod_data_source_block           DMA_hydoughnut-3
_cod_database_code               7117200
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.445
_shelx_estimated_absorpt_t_min   0.445
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N4-C47 = N4-C48
 1.46 with sigma of 0.02
 N4-C46
 1.31 with sigma of 0.02
 C54-C27 = C53-C54 = C52-C53 = C52-C28 = C27-C21 = C28-C21 = C40-C39 = C41-C40
 = C41-C28 = C39-C27
 1.38 with sigma of 0.02
 N6-C36 = N6-C35
 1.47 with sigma of 0.02
 C51-C49 = C51-C50 = N5-C49 = N5-C50
 1.47 with sigma of 0.02
 N7-C56 = N7-C51
 1.47 with sigma of 0.02
 O49-C55
 1.42 with sigma of 0.02
 C47-C46
 2.41 with sigma of 0.04
 C46-C48
 2.41 with sigma of 0.04
 C48-C47
 2.47 with sigma of 0.04
 C52-C21
 2.39 with sigma of 0.04
 C28-C27
 2.39 with sigma of 0.04
 C39-C41
 2.39 with sigma of 0.04
 C53-C28
 2.39 with sigma of 0.04
 C54-C52
 2.39 with sigma of 0.04
 C21-C54
 2.39 with sigma of 0.04
 C27-C53
 2.39 with sigma of 0.04
 C40-C28
 2.39 with sigma of 0.04
 C41-C21
 2.39 with sigma of 0.04
 C21-C39
 2.39 with sigma of 0.04
 C27-C40
 2.39 with sigma of 0.04
 C56-C51
 2.47 with sigma of 0.04
3. Restrained planarity
 C21, C27, C28, C39, C40, C41
 with sigma of 0.1
 C21, C27, C28, C52, C53, C54
 with sigma of 0.1
 O37, N4, C46, C47, C48
 with sigma of 0.1
 C52, C53, C54, O49
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C46: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N2 \\sim C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2 \\sim C35: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C36 \\sim N6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C35 \\sim N6: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N7 \\sim C56: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N7 \\sim C51: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C53 \\sim O49: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O49) \\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: C32(0.75) H32A(0.75) H32B(0.75) H32C(0.75) C33(0.75) H33A(0.75)
 H33B(0.75) H33C(0.75) C34(0.75) H34A(0.75) H34B(0.75) H34C(0.75) N2(0.75)
 H2A(0.75) H2B(0.75) H35A(0.75) H35B(0.75) H35C(0.75) H35D(0.25) H35E(0.25)
 H35F(0.25) H36A(0.75) H36B(0.75) H36C(0.75) H36D(0.25) H36E(0.25) H36F(0.25)
 C39(0.66667) H39(0.66667) C40(0.66667) C41(0.66667) H41(0.66667) O36(0.66667)
 C42(0.66667) H42A(0.66667) H42B(0.66667) H42C(0.66667) C43(0.25) H43A(0.25)
 H43B(0.25) H43C(0.25) C44(0.25) H44A(0.25) H44B(0.25) H44C(0.25) C45(0.25)
 H45A(0.25) H45B(0.25) H45C(0.25) Cl4(0.5) O37(0.5) N4(0.5) C46(0.5) H46(0.5)
 C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5)
 O38(0.5) N5(0.75) H5A(0.75) H5B(0.75) C49(0.75) H49A(0.75) H49B(0.75)
 H49C(0.75) C50(0.75) H50A(0.75) H50B(0.75) H50C(0.75) C51(0.25) H51A(0.25)
 H51B(0.25) H51C(0.25) O39(0.25) O40(0.25) O41(0.25) O42(0.25) O43(0.125)
 O44(0.125) O45(0.125) O46(0.125) O47(0.25) O48(0.125) C52(0.33333)
 H52(0.33333) C53(0.33333) C54(0.33333) H54(0.33333) O49(0.33333) O51(0.5)
 O52(0.5) O53(0.25) O54(0.25) O55(0.25) C55(0.33333) H55A(0.33333)
 H55B(0.33333) H55C(0.33333) N6(0.25) H6A(0.25) H6B(0.25) C56(0.25) H56A(0.25)
 H56B(0.25) H56C(0.25) N7(0.25) H7A(0.25) H7B(0.25)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N5(H5A,H5B), N6(H6A,H6B), N7(H7A,H7B)
6.b Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C35(H35D,H35E,H35F), C36(H36A,
 H36B,H36C), C36(H36D,H36E,H36F), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C16(H16), C19(H19), C20(H20), C21(H21), C24(H24),
 C25(H25), C30(H30), C39(H39), C41(H41), C46(H46), C52(H52), C54(H54)
;
_olex2_submission_special_instructions 'No special instructions were received'