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_7117198
_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         'C64 H32 Cl4 O64 V16, 4(C4 H12 N), 17.5(O)'
_chemical_formula_sum            'C80 H80 Cl4 N4 O81.5 V16'
_chemical_formula_weight         3358.32
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-02-23
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9098(9)
_cell_length_b                   14.9098(9)
_cell_length_c                   38.069(2)
_cell_measurement_reflns_used    7134
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.08
_cell_measurement_theta_min      2.26
_cell_volume                     8462.8(8)
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEX-II CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.518
_diffrn_reflns_av_R_equivalents  0.1153
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            55527
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        15.821
_diffrn_reflns_theta_max         15.821
_diffrn_reflns_theta_min         1.069
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1183 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.8981.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1527
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1473P)^2^+13.2872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2364
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1101
_reflns_number_total             1527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02719e2.cif
_cod_data_source_block           DEA_hydoughnut-1
_cod_original_cell_volume        8462.8(12)
_cod_original_formula_sum        'C80 H80 Cl4 N4 O81.50 V16'
_cod_database_code               7117198
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H13A-H14A
 -2.2 with sigma of 0.02
 N1AA-C13_$3
 1.5 with sigma of 0.02
 C14-C13 = N1AA-C13
 1.5 with sigma of 0.02
 C50_$1-C50_$2
 2.5 with sigma of 0.02
 C50-C52
 1.5 with sigma of 0.02
 N3-C50
 1.47 with sigma of 0.02
 N1AA-C14
 2.5 with sigma of 0.04
 N3-C52
 2.47 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C13 \\sim N1AA \\sim C14: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C50 \\sim C52: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C50 \\sim O1 \\sim O2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Fixed Sof: O11(0.5) Cl1(0.125) O3(0.5) O4(0.5) C12(0.5) O12(0.25) O40(0.25)
 C13(0.25) H13A(0.25) H13B(0.25) N1AA(0.125) H1AA(0.125) H1AB(0.125) C14(0.25)
 H14A(0.25) H14B(0.25) H14C(0.25) C50(0.25) H50B(0.25) H50A(0.25) N3(0.125)
 H3A(0.125) H3B(0.125) C52(0.25) H52A(0.25) H52B(0.25) H52C(0.25) O13(0.01563)
 O14(0.125) O19(0.0625) O20(0.0625) O21(0.03125) O23(0.0625) O24(0.0625)
 O22(0.125) O27(0.03125) O26(0.03125) O29(0.0625) O32(0.01563) O33(0.01563)
 O34(0.03125) O1(0.03125) O2(0.0625) O6(0.0625) O35(0.0625) O36(0.00781)
 O37(0.00781) O39(0.125)
5.a Riding coordinates:
 C13(H13A,H13B), N1AA(H1AA,H1AB), C50(H50B,H50A), N3(H3A,H3B), C52(H52A,H52B,
 H52C)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C10(H10)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'