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_7117199
_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
'C32 H12 Br4 O32 V8, 2(Cl), 5.25(C3 H7 N O), 2(C2 H8 N), 7.33(O0.75)'
_chemical_formula_sum            'C51.75 H64.75 Br4 Cl2 N7.25 O42.75 V8'
_chemical_formula_weight         2270.41
_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   mixed
_audit_creation_date             2015-03-07
_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                103.8173(18)
_cell_angle_beta                 95.3294(16)
_cell_angle_gamma                98.3478(17)
_cell_formula_units_Z            2
_cell_length_a                   15.1975(5)
_cell_length_b                   19.1532(6)
_cell_length_c                   19.3115(6)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.84
_cell_measurement_theta_min      2.38
_cell_volume                     5352.9(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)'
_diffrn_ambient_temperature      100.23
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0878
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            106978
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        59.105
_diffrn_reflns_theta_max         59.105
_diffrn_reflns_theta_min         2.921
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.467
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1313 before and 0.0793 after correction.
The Ratio of minimum to maximum transmission is 0.7376.
The \l/2 correction factor is 0.00150.
;
_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    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         15233
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0982
_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^)+(0.1539P)^2^+50.5301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2603
_refine_ls_wR_factor_ref         0.2992
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9961
_reflns_number_total             15233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02719e2.cif
_cod_data_source_block           DMA_hydoughnut-2
_cod_database_code               7117199
_shelx_estimated_absorpt_t_max   0.551
_shelx_estimated_absorpt_t_min   0.485
_olex2_refinement_description
;
1. Others
 Fixed Sof: C40(0.75) H40A(0.75) H40B(0.75) H40C(0.75) H3AA(0.75) H3AB(0.75)
 H3BC(0.25) H3BD(0.25) H5BC(0.5) H5BD(0.5) H5AA(0.5) H5AB(0.5) N6(0.75)
 C45(0.75) H45A(0.75) H45B(0.75) H45C(0.75) C46(0.75) H46A(0.75) H46B(0.75)
 H46C(0.75) C47(0.75) H47(0.75) O36(0.75) O37(0.5) N7(0.5) C48(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) O38(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) H50C(0.5) N8(0.5) O39(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 H51C(0.5) C52(0.5) H52(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) H54C(0.5) O40(0.25) O41(0.25) O42(0.25) O43(0.25)
 O44(0.25) O45(0.25) O46(0.25) O47(0.25) O48(0.25) O49(0.25) O50(0.25)
 O51(0.25) O52(0.25) O53(0.25) O54(0.125) C55(0.25) H55A(0.25) H55B(0.25)
 H55C(0.25) O55(0.25) O56(0.125) O57(0.25) O58(0.25) C56(0.5) H56(0.5) N9(0.5)
 O59(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) H58(0.5) C59(0.5)
 H59A(0.5) H59B(0.5) H59C(0.5) O61(0.25) O60(0.25)
 Fixed Uiso: H2(0.045) H7(0.062) H10(0.051) H14(0.061) H16(0.047) H18(0.066)
 H20(0.071) H22(0.043) H23(0.052) H24(0.044) H25(0.071) H29(0.046) H33A(0.226)
 H33B(0.226) H33C(0.226) H34A(0.271) H34B(0.271) H34C(0.271) H35(0.222)
 H36A(0.294) H36B(0.294) H36C(0.294) H37A(0.282) H37B(0.282) H37C(0.282)
 H38(0.163) H39A(0.158) H39B(0.158) H39C(0.158) H40A(0.365) H40B(0.365)
 H40C(0.365) H3AA(0.312) H3AB(0.312) H3BC(0.312) H3BD(0.312) H41A(0.301)
 H41B(0.301) H41C(0.301) H42(0.242) H43A(0.384) H43B(0.384) H43C(0.384)
 H44A(0.166) H44B(0.166) H44C(0.166) H5BC(0.281) H5BD(0.281) H5AA(0.281)
 H5AB(0.281) H45A(0.216) H45B(0.216) H45C(0.216) H46A(0.244) H46B(0.244)
 H46C(0.244) H47(0.248) H48A(0.25) H48B(0.25) H48C(0.25) H49A(0.286)
 H49B(0.286) H49C(0.286) H50A(0.167) H50B(0.167) H50C(0.167) H51A(0.39)
 H51B(0.39) H51C(0.39) H52(0.322) H53A(0.151) H53B(0.151) H53C(0.151)
 H54A(0.236) H54B(0.236) H54C(0.236) H55A(0.259) H55B(0.259) H55C(0.259)
 H56(0.086) H57A(0.281) H57B(0.281) H57C(0.281) H58(0.28) H59A(0.44) H59B(0.44)
 H59C(0.44)
 Fixed X: H2(0.9185) H7(0.5826) H10(0.8102) H14(0.5862) H16(0.424) H18(0.6924)
 H20(0.9412) H22(0.7518) H23(0.6836) H24(0.4143) H25(0.8356) H29(0.7598)
 H33A(0.6704) H33B(0.5658) H33C(0.6061) H34A(0.6677) H34B(0.6335) H34C(0.713)
 H35(0.5098) H36A(0.4851) H36B(0.5322) H36C(0.4723) H37A(0.3142) H37B(0.2651)
 H37C(0.3103) H38(0.4688) H39A(0.274) H39B(0.3115) H39C(0.2089) H40A(0.1831)
 H40B(0.183) H40C(0.1133) H3AA(0.2083) H3AB(0.2857) H3BC(0.2707) H3BD(0.1773)
 H41A(1.0712) H41B(1.1645) H41C(1.0959) H42(0.9933) H43A(1.0844) H43B(1.0377)
 H43C(1.142) H44A(0.7639) H44B(0.688) H44C(0.7859) H5BC(0.7838) H5BD(0.7362)
 H5AA(0.8409) H5AB(0.7697) H45A(0.8537) H45B(0.9257) H45C(0.9503) H46A(0.9055)
 H46B(0.9959) H46C(0.9023) H47(1.0004) H48A(0.2474) H48B(0.2446) H48C(0.2302)
 H49A(0.9157) H49B(0.8715) H49C(0.8662) H50A(0.3902) H50B(0.397) H50C(0.3998)
 H51A(0.2073) H51B(0.1736) H51C(0.2653) H52(0.2689) H53A(0.4138) H53B(0.4165)
 H53C(0.4838) H54A(0.6881) H54B(0.7019) H54C(0.7752) H55A(0.2849) H55B(0.2464)
 H55C(0.1789) O56(0.5) H56(0.4451) H57A(0.1936) H57B(0.0951) H57C(0.1548)
 H58(0.2008) H59A(-0.0145) H59B(-0.0272) H59C(0.0016)
 Fixed Y: H2(0.5065) H7(0.2355) H10(0.2926) H14(0.385) H16(0.5354) H18(0.6003)
 H20(0.6802) H22(0.4278) H23(0.1972) H24(0.1447) H25(0.7169) H29(0.8153)
 H33A(0.5709) H33B(0.5401) H33C(0.5545) H34A(0.7368) H34B(0.7436) H34C(0.6993)
 H35(0.7204) H36A(0.1021) H36B(0.0329) H36C(0.0352) H37A(-0.0475) H37B(-0.008)
 H37C(0.0377) H38(0.0198) H39A(0.524) H39B(0.6099) H39C(0.5802) H40A(0.5113)
 H40B(0.4685) H40C(0.5228) H3AA(0.616) H3AB(0.5832) H3BC(0.5516) H3BD(0.5507)
 H41A(0.7886) H41B(0.8432) H41C(0.8577) H42(0.9296) H43A(0.824) H43B(0.8927)
 H43C(0.9048) H44A(0.9367) H44B(0.9602) H44C(0.9588) H5BC(1.073) H5BD(1.0579)
 H5AA(1.0587) H5AB(1.0502) H45A(0.3216) H45B(0.3291) H45C(0.2999) H46A(0.3849)
 H46B(0.444) H46C(0.4667) H47(0.4515) H48A(-0.1519) H48B(-0.2189) H48C(-0.2338)
 H49A(1.0617) H49B(1.1191) H49C(1.0372) H50A(0.0524) H50B(0.1306) H50C(0.0595)
 H51A(-0.0323) H51B(0.0341) H51C(0.0094) H52(0.1) H53A(-0.1684) H53B(-0.1013)
 H53C(-0.158) H54A(1.0637) H54B(1.1222) H54C(1.1263) H55A(0.6841) H55B(0.6458)
 H55C(0.661) O56(0) H56(-0.2345) H57A(0.0872) H57B(0.0837) H57C(0.0247)
 H58(0.0288) H59A(-0.0135) H59B(-0.0066) H59C(-0.0786)
 Fixed Z: H2(0.4342) H7(0.6333) H10(0.3702) H14(0.7849) H16(0.8357)
 H18(0.8475) H20(0.5967) H22(0.2462) H23(0.4428) H24(0.4467) H25(0.7844)
 H29(0.6301) H33A(1.012) H33B(0.9867) H33C(1.0694) H34A(1.1021) H34B(1.0234)
 H34C(1.0344) H35(1.0633) H36A(0.681) H36B(0.6534) H36C(0.7175) H37A(0.6659)
 H37B(0.6131) H37C(0.6922) H38(0.5514) H39A(0.8858) H39B(0.9092) H39C(0.875)
 H40A(1.0387) H40B(0.9566) H40C(0.9768) H3AA(0.99) H3AB(1.0079) H3BC(0.9991)
 H3BD(0.9717) H41A(0.5416) H41B(0.5706) H41C(0.5096) H42(0.5434) H43A(0.6786)
 H43B(0.7092) H43C(0.7) H44A(0.5804) H44B(0.6288) H44C(0.6663) H5BC(0.6702)
 H5BD(0.5974) H5AA(0.6389) H5AB(0.5787) H45A(0.7602) H45B(0.8287) H45C(0.7493)
 H46A(0.6727) H46B(0.696) H46C(0.716) H47(0.8798) H48A(0.1647) H48B(0.0963)
 H48C(0.1729) H49A(0.6305) H49B(0.5967) H49C(0.5495) H50A(-0.0664) H50B(-
 0.0836) H50C(-0.1463) H51A(-0.1197) H51B(-0.0678) H51C(-0.0438) H52(-0.2041)
 H53A(0.084) H53B(0.1524) H53C(0.1545) H54A(0.692) H54B(0.6452) H54C(0.7118)
 H55A(1.0168) H55B(1.0755) H55C(1.0143) O56(0) H56(0.2177) H57A(0.111)
 H57B(0.0716) H57C(0.0391) H58(0.2013) H59A(0.0596) H59B(0.1422) H59C(0.0954)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'