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_7117203
_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
'C6 H15 Cr Mo6 O24, Br, 5(C3 H7 N O), 3(C16 H36 N)'
_chemical_formula_sum            'C69 H158 Br Cr Mo6 N8 O29'
_chemical_formula_weight         2271.59
_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 Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                119.221(4)
_cell_angle_beta                 103.752(3)
_cell_angle_gamma                96.589(3)
_cell_formula_units_Z            1
_cell_length_a                   13.2494(4)
_cell_length_b                   14.7378(6)
_cell_length_c                   14.8892(6)
_cell_measurement_reflns_used    13821
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.2247
_cell_measurement_theta_min      3.0473
_cell_volume                     2371.5(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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -81.00  -53.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -      -15.8208  150.0000  -71.0000 28

  2 omega  -49.00  -23.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -      -15.8208  -37.0000  -60.0000 26

  3 omega   -7.00   26.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       21.1333   77.0000  -60.0000 33

  4 omega  -51.00   46.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       21.1333  -37.0000  -90.0000 97

  5 omega   -6.00   85.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       21.1333   77.0000 -180.0000 91

  6 omega   -2.00   25.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       21.1333  -37.0000  120.0000 27

  7 omega  -49.00   51.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       21.1333  -77.0000   60.0000 100

  8 omega    0.00   40.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -      -15.8208 -122.0000   53.0000 40

  9 omega    4.00   43.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       20.9771  -37.0000   60.0000 39

 10 omega   -4.00   76.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       20.9771 -122.0000 -126.0000 80

 11 omega  -45.00  -19.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       20.9771  -37.0000   60.0000 26

 12 omega   -3.00   81.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       20.9771   37.0000    0.0000 84

 13 omega    1.00   93.00   1.0000    2.9400
omega____ theta____ kappa____ phi______ frames
    -       20.9771   37.0000   90.0000 92
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0038347000
_diffrn_orient_matrix_UB_12      0.0310319000
_diffrn_orient_matrix_UB_13      -0.0243188000
_diffrn_orient_matrix_UB_21      -0.0567453000
_diffrn_orient_matrix_UB_22      -0.0221169000
_diffrn_orient_matrix_UB_23      -0.0228863000
_diffrn_orient_matrix_UB_31      -0.0057215000
_diffrn_orient_matrix_UB_32      0.0426820000
_diffrn_orient_matrix_UB_33      0.0473620000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32552
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.373
_exptl_absorpt_correction_T_max  0.577
_exptl_absorpt_correction_T_min  0.523
_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            pink
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1167
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1051
_refine_ls_number_reflns         18431
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                17114
_reflns_number_total             18431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        2371.54(16)
_cod_database_code               7117203
_audit_block_doi                 10.5517/cc146zht
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.013) H6(0.014) H4(0.012) H5(0.012) H5A(0.026) H5B(0.026)
 H3A(0.021) H3B(0.021) H2A(0.015) H2B(0.015) H1A(0.016) H1B(0.016) H6A(0.048)
 H6B(0.048) H6C(0.048) H64(0.027) H66A(0.036) H66B(0.036) H66C(0.036)
 H65A(0.059) H65B(0.059) H65C(0.059) H67(0.028) H68A(0.037) H68B(0.037)
 H68C(0.037) H69A(0.047) H69B(0.047) H69C(0.047) H61(0.036) H62A(0.059)
 H62B(0.059) H62C(0.059) H63A(0.064) H63B(0.064) H63C(0.064) H55(0.037)
 H56A(0.051) H56B(0.051) H56C(0.051) H57A(0.079) H57B(0.079) H57C(0.079)
 H60(0.037) H58A(0.049) H58B(0.049) H58C(0.049) H59A(0.07) H59B(0.07)
 H59C(0.07) H7A(0.019) H7B(0.019) H8A(0.019) H8B(0.019) H9A(0.023) H9B(0.023)
 H10A(0.041) H10B(0.041) H10C(0.041) H11A(0.02) H11B(0.02) H12A(0.032)
 H12B(0.032) H13A(0.03) H13B(0.03) H14A(0.053) H14B(0.053) H14C(0.053)
 H15A(0.019) H15B(0.019) H16A(0.025) H16B(0.025) H17A(0.03) H17B(0.03)
 H18A(0.044) H18B(0.044) H18C(0.044) H19A(0.023) H19B(0.023) H20A(0.042)
 H20B(0.042) H21A(0.041) H21B(0.041) H22A(0.056) H22B(0.056) H22C(0.056)
 H39A(0.022) H39B(0.022) H40A(0.021) H40B(0.021) H41A(0.025) H41B(0.025)
 H42A(0.035) H42B(0.035) H42C(0.035) H43A(0.023) H43B(0.023) H44A(0.035)
 H44B(0.035) H45A(0.037) H45B(0.037) H46A(0.059) H46B(0.059) H46C(0.059)
 H47A(0.021) H47B(0.021) H48A(0.026) H48B(0.026) H49A(0.03) H49B(0.03)
 H50A(0.044) H50B(0.044) H50C(0.044) H51A(0.023) H51B(0.023) H52A(0.03)
 H52B(0.03) H53A(0.037) H53B(0.037) H54A(0.066) H54B(0.066) H54C(0.066)
 H35A(0.021) H35B(0.021) H36A(0.023) H36B(0.023) H37A(0.025) H37B(0.025)
 H38A(0.042) H38B(0.042) H38C(0.042) H23A(0.018) H23B(0.018) H24A(0.021)
 H24B(0.021) H25A(0.048) H25B(0.048) H26A(0.103) H26B(0.103) H26C(0.103)
 H31A(0.018) H31B(0.018) H32A(0.022) H32B(0.022) H33A(0.025) H33B(0.025)
 H34A(0.045) H34B(0.045) H34C(0.045) H27A(0.019) H27B(0.019) H28A(0.02)
 H28B(0.02) H29A(0.025) H29B(0.025) H30A(0.041) H30B(0.041) H30C(0.041)
 Fixed X: H2(0.0065) H6(0.344) H4(0.331) H5(0.3339) H5A(-0.203) H5B(-0.1943)
 H3A(-0.0301) H3B(-0.0284) H2A(-0.0467) H2B(-0.0512) H1A(-0.0543) H1B(-0.0487)
 H6A(-0.2233) H6B(-0.3043) H6C(-0.1986) H64(0.545) H66A(0.5333) H66B(0.5961)
 H66C(0.4718) H65A(0.5023) H65B(0.6194) H65C(0.6012) H67(-0.1511) H68A(-0.2853)
 H68B(-0.1734) H68C(-0.1788) H69A(-0.1947) H69B(-0.3114) H69C(-0.2257)
 H61(0.6024) H62A(0.5512) H62B(0.4507) H62C(0.5646) H63A(0.5413) H63B(0.5452)
 H63C(0.4379) H55(0.6553) H56A(0.4757) H56B(0.4394) H56C(0.4829) H57A(0.5762)
 H57B(0.6123) H57C(0.6968) H60(0.6703) H58A(0.4976) H58B(0.4245) H58C(0.5293)
 H59A(0.4496) H59B(0.5138) H59C(0.5687) H7A(-0.1448) H7B(-0.0411) H8A(-0.046)
 H8B(-0.1528) H9A(-0.1343) H9B(-0.2412) H10A(-0.249) H10B(-0.2464) H10C(-
 0.1414) H11A(0.0961) H11B(0.1294) H12A(0.1869) H12B(0.1697) H13A(0.318)
 H13B(0.2974) H14A(0.4521) H14B(0.3643) H14C(0.3884) H15A(-0.0055) H15B(-
 0.0554) H16A(-0.2168) H16B(-0.1665) H17A(-0.216) H17B(-0.1493) H18A(-0.3657)
 H18B(-0.2992) H18C(-0.3271) H19A(-0.0745) H19B(0.0348) H20A(0.0166)
 H20B(0.1276) H21A(0.0783) H21B(-0.0056) H22A(0.2171) H22B(0.1318) H22C(0.1509)
 H39A(0.1811) H39B(0.2151) H40A(0.1298) H40B(0.1508) H41A(-0.003) H41B(0.0226)
 H42A(-0.133) H42B(-0.0764) H42C(-0.0428) H43A(0.3336) H43B(0.4469)
 H44A(0.3305) H44B(0.4421) H45A(0.4121) H45B(0.5234) H46A(0.5157) H46B(0.4172)
 H46C(0.5313) H47A(0.397) H47B(0.2893) H48A(0.1881) H48B(0.2937) H49A(0.2282)
 H49B(0.2563) H50A(0.4154) H50B(0.4363) H50C(0.3891) H51A(0.3864) H51B(0.3472)
 H52A(0.5422) H52B(0.5032) H53A(0.564) H53B(0.506) H54A(0.6932) H54B(0.7094)
 H54C(0.652) H35A(0.1206) H35B(0.1202) H36A(0.1649) H36B(0.1652) H37A(0.3421)
 H37B(0.308) H38A(0.2941) H38B(0.4113) H38C(0.3303) H23A(-0.0055) H23B(-0.017)
 H24A(-0.2056) H24B(-0.1858) H25A(-0.1605) H25B(-0.1331) H26A(-0.3021) H26B(-
 0.316) H26C(-0.3432) H31A(-0.0054) H31B(-0.1219) H32A(0.0501) H32B(-0.0704)
 H33A(0.0031) H33B(-0.1202) H34A(-0.1021) H34B(-0.0539) H34C(0.0233) H27A(-
 0.1537) H27B(-0.0498) H28A(-0.1254) H28B(-0.0132) H29A(-0.1358) H29B(-0.1024)
 H30A(-0.3002) H30B(-0.2664) H30C(-0.2864)
 Fixed Y: H2(0.8271) H6(0.714) H4(0.8171) H5(0.9272) H5A(0.6001) H5B(0.5439)
 H3A(0.4346) H3B(0.4966) H2A(0.685) H2B(0.7437) H1A(0.6443) H1B(0.5241)
 H6A(0.3891) H6B(0.4431) H6C(0.4375) H64(0.6523) H66A(0.8053) H66B(0.8349)
 H66C(0.7777) H65A(0.6059) H65B(0.6827) H65C(0.5697) H67(0.9362) H68A(0.8724)
 H68B(0.9517) H68C(0.8381) H69A(1.0973) H69B(1.0268) H69C(1.0639) H61(0.4286)
 H62A(0.6222) H62B(0.6273) H62C(0.7051) H63A(0.5097) H63B(0.6317) H63C(0.5416)
 H55(0.9533) H56A(0.9848) H56B(0.8592) H56C(0.9355) H57A(0.8238) H57B(0.9468)
 H57C(0.8903) H60(1.28) H58A(1.1122) H58B(1.158) H58C(1.2356) H59A(1.0377)
 H59B(0.9851) H59C(1.0372) H7A(0.7632) H7B(0.7886) H8A(0.6045) H8B(0.5803)
 H9A(0.6701) H9B(0.6409) H10A(0.5032) H10B(0.455) H10C(0.4854) H11A(0.6798)
 H11B(0.8) H12A(0.8511) H12B(0.7278) H13A(0.8473) H13B(0.7224) H14A(0.8108)
 H14B(0.7534) H14C(0.8782) H15A(0.7011) H15B(0.6126) H16A(0.6681) H16B(0.7523)
 H17A(0.5249) H17B(0.603) H18A(0.5875) H18B(0.6712) H18C(0.5471) H19A(0.884)
 H19B(0.8881) H20A(0.9641) H20B(0.9622) H21A(1.1334) H21B(1.0748) H22A(1.1079)
 H22B(1.0542) H22C(1.1767) H39A(1.1869) H39B(1.153) H40A(1.331) H40B(1.2813)
 H41A(1.1745) H41B(1.1168) H42A(1.1675) H42B(1.2872) H42C(1.2395) H43A(1.3632)
 H43B(1.3783) H44A(1.1881) H44B(1.1996) H45A(1.3262) H45B(1.341) H46A(1.1589)
 H46B(1.1627) H46C(1.2419) H47A(1.4292) H47B(1.4316) H48A(1.3325) H48B(1.3197)
 H49A(1.4631) H49B(1.5251) H50A(1.474) H50B(1.5523) H50C(1.5858) H51A(1.1585)
 H51B(1.196) H52A(1.3066) H52B(1.341) H53A(1.1491) H53B(1.1659) H54A(1.2075)
 H54B(1.2986) H54C(1.3096) H35A(1.2061) H35B(1.1785) H36A(1.3923) H36B(1.3643)
 H37A(1.4154) H37B(1.3039) H38A(1.2143) H38B(1.2894) H38C(1.3263) H23A(1.3175)
 H23B(1.1969) H24A(1.1626) H24B(1.2885) H25A(1.1577) H25B(1.2839) H26A(1.208)
 H26B(1.2744) H26C(1.1481) H31A(1.3766) H31B(1.2998) H32A(1.2951) H32B(1.2268)
 H33A(1.4569) H33B(1.3956) H34A(1.3168) H34B(1.442) H34C(1.3674) H27A(1.1121)
 H27B(1.0921) H28A(1.03) H28B(1.0198) H29A(0.8534) H29B(0.9014) H30A(0.8944)
 H30B(0.9504) H30C(0.8251)
 Fixed Z: H2(0.8333) H6(0.7539) H4(0.964) H5(0.8491) H5A(0.5901) H5B(0.4735)
 H3A(0.5057) H3B(0.4454) H2A(0.5328) H2B(0.6517) H1A(0.7484) H1B(0.6909)
 H6A(0.4529) H6B(0.509) H6C(0.5784) H64(0.4675) H66A(0.6061) H66B(0.7244)
 H66C(0.6713) H65A(0.679) H65B(0.7506) H65C(0.6458) H67(0.8109) H68A(0.9797)
 H68B(1.0671) H68C(0.9701) H69A(1.027) H69B(0.945) H69C(0.9045) H61(0.8908)
 H62A(1.108) H62B(1.0316) H62C(1.0717) H63A(0.8027) H63B(0.8752) H63C(0.8279)
 H55(1.1526) H56A(1.2638) H56B(1.1817) H56C(1.1461) H57A(1.3008) H57B(1.3929)
 H57C(1.3455) H60(0.9264) H58A(0.9267) H58B(0.8689) H58C(0.9697) H59A(0.6888)
 H59B(0.7445) H59C(0.692) H7A(0.1283) H7B(0.1026) H8A(0.0151) H8B(0.0376) H9A(-
 0.0898) H9B(-0.0701) H10A(-0.2436) H10B(-0.1698) H10C(-0.1917) H11A(0.1675)
 H11B(0.2001) H12A(0.3888) H12B(0.3459) H13A(0.3088) H13B(0.2574) H14A(0.4099)
 H14B(0.4338) H14C(0.483) H15A(0.3247) H15B(0.1998) H16A(0.1948) H16B(0.3215)
 H17A(0.2196) H17B(0.3444) H18A(0.2471) H18B(0.371) H18C(0.3259) H19A(0.3168)
 H19B(0.3897) H20A(0.2476) H20B(0.3131) H21A(0.3987) H21B(0.425) H22A(0.5057)
 H22B(0.5349) H22C(0.5743) H39A(1.1755) H39B(1.2602) H40A(1.3067) H40B(1.3796)
 H41A(1.1669) H41B(1.231) H42A(1.2492) H42B(1.2916) H42C(1.3645) H43A(1.4583)
 H43B(1.4453) H44A(1.4176) H44B(1.3995) H45A(1.602) H45B(1.5846) H46A(1.5414)
 H46B(1.5829) H46C(1.6641) H47A(1.319) H47B(1.345) H48A(1.1587) H48B(1.1286)
 H49A(1.1204) H49B(1.2475) H50A(1.1503) H50B(1.2753) H50C(1.1924) H51A(1.2335)
 H51B(1.1526) H52A(1.3324) H52B(1.2483) H53A(1.2007) H53B(1.1073) H54A(1.1462)
 H54B(1.2664) H54C(1.1685) H35A(0.8542) H35B(0.7383) H36A(0.9184) H36B(0.8023)
 H37A(0.9357) H37B(0.9244) H38A(0.7391) H38B(0.814) H38C(0.7518) H23A(0.7065)
 H23B(0.6208) H24A(0.6109) H24B(0.671) H25A(0.467) H25B(0.528) H26A(0.3923)
 H26B(0.5067) H26C(0.4449) H31A(0.885) H31B(0.8349) H32A(0.9853) H32B(0.9403)
 H33A(1.0765) H33B(1.0215) H34A(1.1252) H34B(1.2057) H34C(1.1744) H27A(0.7292)
 H27B(0.7841) H28A(0.5627) H28B(0.616) H29A(0.5285) H29B(0.6544) H30A(0.525)
 H30B(0.6523) H30C(0.5779)
;