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_7117204
_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_formula_moiety
'C5 H13 Cr Mo6 O25, 2(C16 H36 N), 3(C3 H7 N O), H2 O'
_chemical_formula_sum            'C46 H108 Cr Mo6 N5 O28'
_chemical_formula_weight         1807.00
_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
_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                86.727(4)
_cell_angle_beta                 83.692(4)
_cell_angle_gamma                62.304(6)
_cell_formula_units_Z            2
_cell_length_a                   13.6865(8)
_cell_length_b                   13.7366(8)
_cell_length_c                   21.5248(9)
_cell_measurement_reflns_used    13961
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.688
_cell_measurement_theta_min      0.555
_cell_volume                     3561.4(4)
_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      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30186
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.7061
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     819
_refine_ls_number_reflns         13961
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0211P)^2^+7.9358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                11643
_reflns_number_total             13961
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        3561.3(3)
_cod_database_code               7117204
_audit_block_doi                 10.5517/cc146zjv
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H18A(0.021) H18B(0.021) H20A(0.025) H20B(0.025) H19A(0.023)
 H19B(0.023) H22A(0.028) H22B(0.028) H10A(0.024) H10B(0.024) H23A(0.035)
 H23B(0.035) H5A(0.034) H5B(0.034) H8A(0.03) H8B(0.03) H6A(0.022) H6B(0.022)
 H25(0.136) H3A(0.027) H3B(0.027) H15A(0.032) H15B(0.032) H24A(0.044)
 H24B(0.044) H7A(0.027) H7B(0.027) H14A(0.027) H14B(0.027) H21A(0.045)
 H21B(0.045) H21C(0.045) H2A(0.022) H2B(0.022) H1A(0.024) H1B(0.024) H55(0.044)
 H25A(0.072) H25B(0.072) H25C(0.072) H30A(0.036) H30B(0.036) H9A(0.053)
 H9B(0.053) H9C(0.053) H33A(0.063) H33B(0.063) H33C(0.063) H16A(0.053)
 H16B(0.053) H31A(0.033) H31B(0.033) H32A(0.037) H32B(0.037) H17A(0.075)
 H17B(0.075) H17C(0.075) H26A(0.059) H26B(0.059) H42A(0.031) H42B(0.031)
 H56A(0.075) H56B(0.075) H56C(0.075) H45A(0.031) H45B(0.031) H27A(0.09)
 H27B(0.09) H11A(0.035) H11B(0.035) H50(0.035) H51A(0.057) H51B(0.057)
 H51C(0.057) H52A(0.051) H52B(0.051) H52C(0.051) H47A(0.075) H47B(0.075)
 H47C(0.075) H13A(0.062) H13B(0.062) H13C(0.062) H12A(0.068) H12B(0.068)
 H44A(0.039) H44B(0.039) H44C(0.039) H46(0.063) H40A(0.031) H40B(0.031)
 H28A(0.126) H28B(0.126) H29A(0.154) H29B(0.154) H29C(0.154) H53A(0.094)
 H53B(0.094) H53C(0.094) H49A(0.105) H49B(0.105) H49C(0.105) H29D(0.105)
 H29E(0.105) H37A(0.055) H37B(0.055) H37C(0.055) H43A(0.044) H43B(0.044)
 H39A(0.044) H39B(0.044) H54A(0.094) H54B(0.094) H54C(0.094) H48A(0.105)
 H48B(0.105) H48C(0.105) H38A(0.044) H38B(0.044)
 Fixed X: H5(0.6236) H4(0.6161) H2(0.3572) H6(0.4355) H18A(0.9698)
 H18B(1.0192) H20A(0.998) H20B(1.0595) H19A(0.8359) H19B(0.8945) H22A(-0.0313)
 H22B(0.0169) H10A(0.803) H10B(0.7314) H23A(0.097) H23B(0.1471) H5A(0.4809)
 H5B(0.3817) H8A(0.9674) H8B(1.0853) H6A(0.8884) H6B(1.0002) H25(0.3657)
 H3A(0.598) H3B(0.4975) H15A(0.9709) H15B(0.9625) H24A(-0.0778) H24B(-0.0203)
 H7A(0.9117) H7B(1.0294) H14A(0.7855) H14B(0.7842) H21A(0.938) H21B(1.0019)
 H21C(0.8787) H2A(0.3236) H2B(0.3192) H1A(0.4831) H1B(0.5887) H55(0.4378)
 H25A(0.086) H25B(-0.0397) H25C(0.0342) H30A(-0.0161) H30B(0.0955) H9A(1.118)
 H9B(1.0902) H9C(0.9997) H33A(-0.0158) H33B(-0.1113) H33C(-0.1306) H16A(0.823)
 H16B(0.8218) H31A(-0.0388) H31B(0.0787) H32A(-0.0979) H32B(0.0186)
 H17A(0.9169) H17B(0.9974) H17C(1.0016) H26A(0.1999) H26B(0.1965) H42A(0.1944)
 H42B(0.2631) H56A(0.3119) H56B(0.2826) H56C(0.2068) H45A(0.2932) H45B(0.2382)
 H27A(0.0155) H27B(0.018) H11A(0.6673) H11B(0.7385) H50(0.4023) H51A(0.3387)
 H51B(0.3599) H51C(0.2447) H52A(0.314) H52B(0.4355) H52C(0.4104) H47A(0.1745)
 H47B(0.2803) H47C(0.2267) H13A(0.4992) H13B(0.464) H13C(0.5619) H12A(0.6374)
 H12B(0.5632) H44A(0.3322) H44B(0.3402) H44C(0.4478) H46(0.3777) H40A(0.4368)
 H40B(0.4286) H28A(0.0513) H28B(0.1642) H29A(0.2295) H29B(0.1146) H29C(0.189)
 H53A(0.269) H53B(0.3326) H53C(0.3985) H49A(0.3408) H49B(0.4462) H49C(0.4065)
 H37A(0.4917) H37B(0.5251) H37C(0.4562) H43A(0.3105) H43B(0.3773) H39A(0.2767)
 H39B(0.3575) H54A(0.2147) H54B(0.246) H54C(0.3169) H48A(0.2204) H48B(0.317)
 H48C(0.343) H38A(0.2364) H38B(0.1706)
 Fixed Y: H5(0.1186) H4(0.3283) H2(0.4315) H6(0.2983) H18A(-0.3391) H18B(-
 0.4256) H20A(-0.1981) H20B(-0.287) H19A(-0.2165) H19B(-0.3023) H22A(-0.026)
 H22B(-0.1098) H10A(-0.2942) H10B(-0.2666) H23A(-0.1547) H23B(-0.2389)
 H5A(0.1591) H5B(0.2703) H8A(-0.6292) H8B(-0.6593) H6A(-0.55) H6B(-0.5668)
 H25(0.0819) H3A(0.0243) H3B(0.0108) H15A(-0.4967) H15B(-0.5958) H24A(-0.1533)
 H24B(-0.2457) H7A(-0.4398) H7B(-0.471) H14A(-0.4804) H14B(-0.3811) H21A(-
 0.1679) H21B(-0.1125) H21C(-0.0788) H2A(0.1781) H2B(0.2943) H1A(0.3143)
 H1B(0.2104) H55(0.0834) H25A(-0.3667) H25B(-0.319) H25C(-0.2743) H30A(0.116)
 H30B(0.1031) H9A(-0.5684) H9B(-0.66) H9C(-0.5365) H33A(0.0909) H33B(0.212)
 H33C(0.1151) H16A(-0.5778) H16B(-0.4728) H31A(0.0201) H31B(-0.0069)
 H32A(0.2105) H32B(0.1811) H17A(-0.6194) H17B(-0.6868) H17C(-0.5825) H26A(-
 0.0684) H26B(0.0328) H42A(-0.1509) H42B(-0.1708) H56A(0.0272) H56B(0.0278)
 H56C(0.1267) H45A(-0.0159) H45B(-0.0135) H27A(0.041) H27B(0.1424) H11A(-
 0.3928) H11B(-0.4191) H50(0.5105) H51A(0.6932) H51B(0.6061) H51C(0.6631)
 H52A(0.4413) H52B(0.4129) H52C(0.3879) H47A(0.6186) H47B(0.525) H47C(0.4988)
 H13A(-0.3296) H13B(-0.2197) H13C(-0.3293) H12A(-0.2324) H12B(-0.2119) H44A(-
 0.1654) H44B(-0.2571) H44C(-0.2648) H46(0.5619) H40A(-0.1182) H40B(-0.2014)
 H28A(0.1551) H28B(0.1214) H29A(-0.0593) H29B(-0.0315) H29C(0.0166)
 H53A(0.2366) H53B(0.1151) H53C(0.1795) H49A(0.6931) H49B(0.6037) H49C(0.5756)
 H37A(-0.2226) H37B(-0.2298) H37C(-0.1148) H43A(-0.1677) H43B(-0.2668) H39A(-
 0.0425) H39B(-0.1347) H54A(0.275) H54B(0.236) H54C(0.2788) H48A(0.7471)
 H48B(0.7236) H48C(0.6966) H38A(-0.1978) H38B(-0.1493)
 Fixed Z: H5(0.1764) H4(0.1738) H2(0.3261) H6(0.138) H18A(0.239) H18B(0.1852)
 H20A(0.1764) H20B(0.1241) H19A(0.173) H19B(0.1188) H22A(0.3205) H22B(0.2654)
 H10A(0.2956) H10B(0.2392) H23A(0.3844) H23B(0.3289) H5A(0.4894) H5B(0.4719)
 H8A(0.3739) H8B(0.34) H6A(0.2791) H6B(0.2424) H25(0.4795) H3A(0.4125)
 H3B(0.3938) H15A(0.1134) H15B(0.1492) H24A(0.3787) H24B(0.3282) H7A(0.3523)
 H7B(0.3174) H14A(0.1927) H14B(0.1528) H21A(0.0526) H21B(0.0794) H21C(0.1049)
 H2A(0.3656) H2B(0.3635) H1A(0.3933) H1B(0.4129) H55(0.0808) H25A(0.401)
 H25B(0.4256) H25C(0.4517) H30A(0.2642) H30B(0.2291) H9A(0.4176) H9B(0.4482)
 H9C(0.4512) H33A(0.0542) H33B(0.06) H33C(0.0904) H16A(0.0896) H16B(0.0565)
 H31A(0.1874) H31B(0.1538) H32A(0.1667) H32B(0.1312) H17A(-0.0105) H17B(0.0401)
 H17C(0.0092) H26A(0.3542) H26B(0.3156) H42A(0.2103) H42B(0.2675) H56A(0.0684)
 H56B(0) H56C(0.0444) H45A(0.232) H45B(0.1711) H27A(0.3946) H27B(0.3584)
 H11A(0.2777) H11B(0.3347) H50(-0.1004) H51A(0.0167) H51B(0.0707) H51C(0.0431)
 H52A(0.0285) H52B(0.0401) H52C(-0.0248) H47A(0.5362) H47B(0.5633) H47C(0.51)
 H13A(0.3618) H13B(0.3969) H13C(0.4185) H12A(0.3637) H12B(0.3093) H44A(0.0944)
 H44B(0.1435) H44C(0.1051) H46(0.3953) H40A(0.158) H40B(0.2087) H28A(0.4583)
 H28B(0.4175) H29A(0.4514) H29B(0.4885) H29C(0.5103) H53A(-0.0584) H53B(-
 0.0822) H53C(-0.0716) H49A(0.5195) H49B(0.4817) H49C(0.5483) H37A(0.08)
 H37B(0.1481) H37C(0.1173) H43A(0.1142) H43B(0.1579) H39A(0.1911) H39B(0.2336)
 H54A(0.0223) H54B(-0.0474) H54C(-0.0162) H48A(0.5027) H48B(0.4499)
 H48C(0.5198) H38A(0.2636) H38B(0.2051)
;