Unprecedented chi isomers of single-side triol-functionalized Anderson polyoxometalates and their proton-controlled isomer transformation
Jiangwei Zhang; Zhenhua Liu; Yichao Huang; Jin zhang; Jian Hao; Yongge Wei; Chem.Commun. 51 (2015) 9097–; doi:10.1039/C5cc02947C

data_7117205
_publ_section_title
;
 Unprecedented chi isomers of single-side triol-functionalized Anderson
 polyoxometalates and their proton-controlled isomer transformation
;
_journal_name_full               Chem.Commun.
_journal_page_first              9097
_journal_paper_doi               10.1039/C5cc02947C
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C4 H12 Mn Mo6 N O24, Br, 3(C16 H36 N), 5(C3 H7 N O)'
_chemical_formula_sum            'C67 H155 Br Mn Mo6 N9 O29'
_chemical_formula_weight         2261.47
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                119.330(4)
_cell_angle_beta                 103.729(3)
_cell_angle_gamma                96.883(3)
_cell_formula_units_Z            1
_cell_length_a                   13.2671(5)
_cell_length_b                   14.7560(6)
_cell_length_c                   14.8870(4)
_cell_measurement_reflns_used    7915
_cell_measurement_temperature    109(6)
_cell_measurement_theta_max      29.2286
_cell_measurement_theta_min      3.0447
_cell_volume                     2370.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      109(6)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
  1 omega  -18.00    8.00   1.0000    2.9700
omega____ theta____ kappa____ phi______ frames
    -      -15.9950  -77.0000  -30.0000 26

  2 omega   -9.00   88.00   1.0000    2.9700
omega____ theta____ kappa____ phi______ frames
    -       21.1513   77.0000  -30.0000 97

  3 omega   -1.00   88.00   1.0000    2.9700
omega____ theta____ kappa____ phi______ frames
    -       21.1513   77.0000  120.0000 89

  4 omega  -47.00   46.00   1.0000    2.9700
omega____ theta____ kappa____ phi______ frames
    -       21.1513  -77.0000 -150.0000 93

  5 omega    5.00   92.00   1.0000    2.9700
omega____ theta____ kappa____ phi______ frames
    -       21.1513   37.0000  120.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0356217000
_diffrn_orient_matrix_UB_12      0.0451228000
_diffrn_orient_matrix_UB_13      0.0077836000
_diffrn_orient_matrix_UB_21      -0.0257129000
_diffrn_orient_matrix_UB_22      -0.0174217000
_diffrn_orient_matrix_UB_23      -0.0555477000
_diffrn_orient_matrix_UB_31      -0.0367977000
_diffrn_orient_matrix_UB_32      0.0309290000
_diffrn_orient_matrix_UB_33      0.0153717000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19084
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.573
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1056
_refine_ls_number_reflns         13556
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                12680
_reflns_number_total             13556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        2370.38(14)
_cod_database_code               7117205
_audit_block_doi                 10.5517/cc146zkw
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{H34C, H34A}
2. Others
 Fixed Uiso: H2A(0.015) H2B(0.015) H3A(0.021) H3B(0.021) H1A(0.015) H1B(0.015)
 H29A(0.018) H29B(0.018) H33A(0.022) H33B(0.022) H22A(0.019) H22B(0.019)
 H23A(0.022) H23B(0.022) H62A(0.07) H62B(0.07) H62C(0.07) H39A(0.018)
 H39B(0.018) H9A(0.017) H9B(0.017) H10A(0.021) H10B(0.021) H47A(0.02)
 H47B(0.02) H13A(0.017) H13B(0.017) H14A(0.019) H14B(0.019) H17A(0.023)
 H17B(0.023) H40(0.022) H18A(0.019) H18B(0.019) H21A(0.017) H21B(0.017)
 H15A(0.024) H15B(0.024) H5A(0.017) H5B(0.017) H51A(0.021) H51B(0.021)
 H24A(0.04) H24B(0.04) H24C(0.04) H6A(0.022) H6B(0.022) H49A(0.029) H49B(0.029)
 H7A(0.026) H7B(0.026) H48A(0.024) H48B(0.024) H41A(0.023) H41B(0.023)
 H26A(0.023) H26B(0.023) H52A(0.026) H52B(0.026) H43A(0.023) H43B(0.023)
 H25A(0.02) H25B(0.02) H67(0.031) H19A(0.028) H19B(0.028) H44A(0.031)
 H44B(0.031) H50A(0.048) H50B(0.048) H50C(0.048) H63A(0.047) H63B(0.047)
 H63C(0.047) H27A(0.029) H27B(0.029) H1C(0.064) H1D(0.064) H16A(0.043)
 H16B(0.043) H16C(0.043) H53A(0.033) H53B(0.033) H68A(0.044) H68B(0.044)
 H68C(0.044) H61(0.033) H64(0.041) H45A(0.037) H45B(0.037) H20A(0.042)
 H20B(0.042) H20C(0.042) H31A(0.032) H31B(0.032) H30A(0.031) H30B(0.031)
 H8A(0.045) H8B(0.045) H8C(0.045) H28A(0.05) H28B(0.05) H28C(0.05) H42A(0.037)
 H42B(0.037) H42C(0.037) H11A(0.036) H11B(0.036) H69A(0.045) H69B(0.045)
 H69C(0.045) H55(0.042) H58(0.041) H66A(0.052) H66B(0.052) H66C(0.052)
 H32A(0.054) H32B(0.054) H32C(0.054) H57A(0.056) H57B(0.056) H57C(0.056)
 H36A(0.032) H36B(0.032) H34A(0.042) H34B(0.042) H34C(0.042) H34D(0.042)
 H54A(0.058) H54B(0.058) H54C(0.058) H12A(0.058) H12B(0.058) H12C(0.058)
 H60A(0.072) H60B(0.072) H60C(0.072) H65A(0.081) H65B(0.081) H65C(0.081)
 H59A(0.08) H59B(0.08) H59C(0.08) H56A(0.071) H56B(0.071) H56C(0.071)
 H46A(0.062) H46B(0.062) H46C(0.062) H37A(0.04) H37B(0.04) H37C(0.04)
 H35A(0.032) H35B(0.032) H38A(0.04) H38B(0.04) H38C(0.04)
 Fixed X: H5(-0.166) H6(-0.1553) H1(0.172) H4(-0.1534) H2A(0.2262) H2B(0.2329)
 H3A(0.2066) H3B(0.2078) H1A(0.2297) H1B(0.2254) H29A(0.0486) H29B(0.0816)
 H33A(0.1436) H33B(0.2529) H22A(0.2255) H22B(0.3333) H23A(0.3107) H23B(0.4188)
 H62A(-0.4428) H62B(-0.3259) H62C(-0.4254) H39A(-0.0412) H39B(-0.0073)
 H9A(0.1939) H9B(0.1817) H10A(0.3823) H10B(0.3637) H47A(-0.1134) H47B(-0.2216)
 H13A(0.2991) H13B(0.1823) H14A(0.2488) H14B(0.1276) H17A(0.0126) H17B(0.0125)
 H18A(0.0579) H18B(0.0586) H21A(0.2182) H21B(0.3221) H15A(0.2948) H15B(0.1708)
 H5A(0.2279) H5B(0.3318) H51A(-0.2125) H51B(-0.1713) H24A(0.4272) H24B(0.319)
 H24C(0.4232) H6A(0.3031) H6B(0.1913) H49A(-0.0489) H49B(-0.0795) H7A(0.2814)
 H7B(0.317) H48A(-0.1205) H48B(-0.0137) H41A(0.1519) H41B(0.1786) H26A(0.3952)
 H26B(0.3452) H52A(-0.3679) H52B(-0.3272) H43A(-0.2716) H43B(-0.1579)
 H25A(0.233) H25B(0.1834) H67(0.3283) H19A(-0.1325) H19B(-0.1658) H44A(-0.2672)
 H44B(-0.1546) H50A(-0.2379) H50B(-0.2145) H50C(-0.2631) H63A(-0.2917) H63B(-
 0.4154) H63C(-0.3624) H27A(0.3272) H27B(0.3943) H16A(0.2774) H16B(0.152)
 H16C(0.23) H53A(-0.3312) H53B(-0.389) H68A(0.3539) H68B(0.3525) H68C(0.4626)
 H61(-0.3694) H64(-0.4791) H45A(-0.346) H45B(-0.2337) H20A(-0.1181) H20B(-
 0.1511) H20C(-0.2349) H31A(-0.1193) H31B(-0.1402) H30A(0.0079) H30B(-0.0097)
 H8A(0.4793) H8B(0.4677) H8C(0.4433) H28A(0.5433) H28B(0.5072) H28C(0.4762)
 H42A(0.3096) H42B(0.2193) H42C(0.2518) H11A(0.3052) H11B(0.3357) H69A(0.3718)
 H69B(0.4004) H69C(0.4881) H55(-0.4943) H58(-0.4254) H66A(-0.3084) H66B(-
 0.2638) H66C(-0.2972) H32A(-0.2762) H32B(-0.2053) H32C(-0.192) H57A(-0.3243)
 H57B(-0.3504) H57C(-0.2465) H36A(0.1829) H36B(0.0955) H34A(0.0506)
 H34B(0.1614) H34C(0.0516) H34D(0.1645) H54A(-0.5187) H54B(-0.4771) H54C(-
 0.5346) H12A(0.475) H12B(0.5186) H12C(0.4877) H60A(-0.2731) H60B(-0.3771)
 H60C(-0.384) H65A(-0.4057) H65B(-0.522) H65C(-0.4268) H59A(-0.3613) H59B(-
 0.2619) H59C(-0.3721) H56A(-0.3865) H56B(-0.3399) H56C(-0.2689) H46A(-0.3507)
 H46B(-0.3417) H46C(-0.2392) H37A(-0.0396) H37B(0.0229) H37C(0.0489)
 H35A(0.1129) H35B(0.18) H38A(0.0149) H38B(0.021) H38C(-0.0478)
 Fixed Y: H5(0.0588) H6(-0.1548) H1(-0.0513) H4(-0.0453) H2A(0.2532)
 H2B(0.1334) H3A(0.2816) H3B(0.343) H1A(0.0336) H1B(0.0913) H29A(-0.0264)
 H29B(0.0942) H33A(-0.1114) H33B(-0.1066) H22A(0.1723) H22B(0.1952)
 H23A(0.1061) H23B(0.1353) H62A(0.0861) H62B(0.1646) H62C(0.2009) H39A(-0.38)
 H39B(-0.4108) H9A(-0.4239) H9B(-0.5445) H10A(-0.3861) H10B(-0.5122) H47A(-
 0.6584) H47B(-0.6576) H13A(-0.5247) H13B(-0.6019) H14A(-0.4525) H14B(-0.5195)
 H17A(-0.5893) H17B(-0.6171) H18A(-0.4031) H18B(-0.4311) H21A(-0.0134)
 H21B(0.0113) H15A(-0.622) H15B(-0.6819) H5A(-0.3167) H5B(-0.3362) H51A(-
 0.3857) H51B(-0.4201) H24A(0.2717) H24B(0.2886) H24C(0.3201) H6A(-0.2549) H6B(-
 0.245) H49A(-0.6892) H49B(-0.7514) H7A(-0.1241) H7B(-0.0768) H48A(-0.5478)
 H48B(-0.5561) H41A(-0.3414) H41B(-0.3966) H26A(0.1088) H26B(0.025) H52A(-
 0.5376) H52B(-0.5671) H43A(-0.6057) H43B(-0.5894) H25A(0.1626) H25B(0.0735)
 H67(-0.1598) H19A(-0.5305) H19B(-0.6422) H44A(-0.4265) H44B(-0.4128) H50A(-
 0.7025) H50B(-0.8157) H50C(-0.7772) H63A(-0.0009) H63B(-0.0597) H63C(-0.0326)
 H27A(0.1751) H27B(0.2529) H16A(-0.5414) H16B(-0.5937) H16C(-0.6671) H53A(-
 0.3904) H53B(-0.3767) H68A(-0.0653) H68B(-0.1783) H68C(-0.0954) H61(0.1224)
 H64(-0.1811) H45A(-0.5684) H45B(-0.5501) H20A(-0.441) H20B(-0.5527) H20C(-
 0.5189) H31A(0.0504) H31B(-0.0745) H30A(0.0459) H30B(-0.0775) H8A(-0.1233)
 H8B(-0.05) H8C(-0.1755) H28A(0.1878) H28B(0.2329) H28C(0.1077) H42A(-0.3919)
 H42B(-0.4638) H42C(-0.5118) H11A(-0.5213) H11B(-0.3945) H69A(-0.3209) H69B(-
 0.2892) H69C(-0.2503) H55(-0.5051) H58(-0.6584) H66A(-0.1726) H66B(-0.0852)
 H66C(-0.2085) H32A(-0.0475) H32B(-0.1008) H32C(0.0239) H57A(-0.3437) H57B(-
 0.4656) H57C(-0.3814) H36A(-0.3047) H36B(-0.3598) H34A(-0.1891) H34B(-0.1894)
 H34C(-0.1899) H34D(-0.1989) H54A(-0.4359) H54B(-0.5375) H54C(-0.5267) H12A(-
 0.4518) H12B(-0.3871) H12C(-0.5139) H60A(-0.8508) H60B(-0.8521) H60C(-0.9331)
 H65A(-0.0516) H65B(-0.1311) H65C(-0.1735) H59A(-0.7387) H59B(-0.7757) H59C(-
 0.8621) H56A(-0.2645) H56B(-0.2127) H56C(-0.2624) H46A(-0.3938) H46B(-0.4639)
 H46C(-0.3769) H37A(-0.3296) H37B(-0.403) H37C(-0.28) H35A(-0.2666) H35B(-
 0.3144) H38A(-0.4075) H38B(-0.4468) H38C(-0.3671)
 Fixed Z: H5(-0.4596) H6(-0.5546) H1(-0.5381) H4(-0.6698) H2A(-0.3951) H2B(-
 0.4528) H3A(-0.148) H3B(-0.2089) H1A(-0.3567) H1B(-0.2375) H29A(-0.905) H29B(-
 0.8716) H33A(-1.0941) H33B(-1.021) H22A(-0.7196) H22B(-0.741) H23A(-0.6135)
 H23B(-0.6314) H62A(-0.4596) H62B(-0.3881) H62C(-0.357) H39A(-0.9688) H39B(-
 0.8817) H9A(-0.3256) H9B(-0.4126) H10A(-0.3109) H10B(-0.379) H47A(-1.052)
 H47B(-1.0271) H13A(-0.5403) H13B(-0.5908) H14A(-0.6467) H14B(-0.6913) H17A(-
 0.5085) H17B(-0.6247) H18A(-0.444) H18B(-0.5597) H21A(-0.8073) H21B(-0.8331)
 H15A(-0.7283) H15B(-0.783) H5A(-0.487) H5B(-0.4319) H51A(-0.9419) H51B(-
 0.8589) H24A(-0.4599) H24B(-0.511) H24C(-0.5334) H6A(-0.2659) H6B(-0.3196)
 H49A(-0.8285) H49B(-0.9563) H7A(-0.3559) H7B(-0.2297) H48A(-0.8368) H48B(-
 0.8647) H41A(-0.9371) H41B(-0.8707) H26A(-0.8986) H26B(-1.0258) H52A(-1.0394)
 H52B(-0.9515) H43A(-1.1535) H43B(-1.1653) H25A(-0.9043) H25B(-1.0295) H67(-
 0.5152) H19A(-0.631) H19B(-0.6426) H44A(-1.1063) H44B(-1.1219) H50A(-0.8537)
 H50B(-0.9026) H50C(-0.9803) H63A(-0.3708) H63B(-0.4338) H63C(-0.3144) H27A(-
 1.0466) H27B(-0.9213) H16A(-0.8306) H16B(-0.8812) H16C(-0.9116) H53A(-0.8142)
 H53B(-0.91) H68A(-0.6764) H68B(-0.7717) H68C(-0.682) H61(-0.1754) H64(-0.8595)
 H45A(-1.2936) H45B(-1.3084) H20A(-0.4465) H20B(-0.4579) H20C(-0.5208) H31A(-
 0.9633) H31B(-1.0154) H30A(-1.0506) H30B(-1.0939) H8A(-0.2316) H8B(-0.2799)
 H8C(-0.3588) H28A(-0.9505) H28B(-1.0252) H28C(-1.0755) H42A(-0.9536) H42B(-
 1.0695) H42C(-0.9969) H11A(-0.2427) H11B(-0.173) H69A(-0.7323) H69B(-0.6103)
 H69C(-0.6478) H55(-0.6326) H58(-0.595) H66A(-0.8595) H66B(-0.8819) H66C(-
 0.9738) H32A(-1.1205) H32B(-1.1916) H32C(-1.135) H57A(-0.6383) H57B(-0.6745)
 H57C(-0.5747) H36A(-1.1289) H36B(-1.1025) H34A(-1.0204) H34B(-0.9539) H34C(-
 1.0162) H34D(-0.9609) H54A(-0.8545) H54B(-0.8772) H54C(-0.975) H12A(-0.106)
 H12B(-0.1531) H12C(-0.2215) H60A(-0.7386) H60B(-0.8162) H60C(-0.7771) H65A(-
 1.0064) H65B(-1.0609) H65C(-1.097) H59A(-0.5099) H59B(-0.5403) H59C(-0.5859)
 H56A(-0.3965) H56B(-0.4536) H56C(-0.3994) H46A(-1.255) H46B(-1.3714) H46C(-
 1.2716) H37A(-1.211) H37B(-1.2806) H37C(-1.2404) H35A(-1.1829) H35B(-1.1238)
 H38A(-1.1314) H38B(-1.2483) H38C(-1.2016)
;