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_7117201
_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
'C4 H12 Cr Mo6 N O24, 2(H2 O), 3(C3 H7 N O), 2(C16 H36 N)'
_chemical_formula_sum            'C45 H109 Cr Mo6 N6 O29'
_chemical_formula_weight         1826.00
_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                86.768(7)
_cell_angle_beta                 88.944(8)
_cell_angle_gamma                63.016(9)
_cell_formula_units_Z            2
_cell_length_a                   13.5540(14)
_cell_length_b                   13.7899(10)
_cell_length_c                   21.0955(18)
_cell_measurement_reflns_used    11106
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1721
_cell_measurement_theta_min      3.0600
_cell_volume                     3508.0(6)
_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      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_details
;
  1 omega  -72.00  -30.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -15.9711  -37.0000  -90.0000 42

  2 omega  -15.00   10.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -15.9711  -37.0000  120.0000 25

  3 omega  -41.00  -11.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      -15.9711   77.0000 -180.0000 30

  4 omega  -10.00   88.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.2836   79.0000  106.0000 98

  5 omega    3.00   80.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.2836    0.0000  -30.0000 77

  6 omega    5.00   32.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.2836   37.0000   90.0000 27

  7 omega   -8.00   86.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.2836   77.0000  -30.0000 94

  8 omega  -48.00   47.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -       21.2836  -77.0000 -150.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0434007000
_diffrn_orient_matrix_UB_12      0.0362980000
_diffrn_orient_matrix_UB_13      -0.0205620000
_diffrn_orient_matrix_UB_21      -0.0391720000
_diffrn_orient_matrix_UB_22      -0.0070734000
_diffrn_orient_matrix_UB_23      0.0199442000
_diffrn_orient_matrix_UB_31      -0.0053712000
_diffrn_orient_matrix_UB_32      0.0443838000
_diffrn_orient_matrix_UB_33      0.0176501000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30886
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.429
_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    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         13739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                11502
_reflns_number_total             13739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        3508.0(5)
_cod_database_code               7117201
_audit_block_doi                 10.5517/cc146zfr
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Sof: O28(0.7) H28D(0.7) H28E(0.7)
 Fixed Uiso: H29C(0.047) H29D(0.047) H2A(0.023) H2B(0.023) H14A(0.019)
 H14B(0.019) H13A(0.018) H13B(0.018) H6A(0.02) H6B(0.02) H5A(0.019) H5B(0.019)
 H15A(0.022) H15B(0.022) H1A(0.018) H1B(0.018) H30A(0.024) H30B(0.024)
 H31A(0.027) H31B(0.027) H1C(0.058) H1D(0.058) H27A(0.028) H27B(0.028)
 H33A(0.026) H33B(0.026) H3A(0.019) H3B(0.019) H17A(0.018) H17B(0.018)
 H9A(0.018) H9B(0.018) H28A(0.045) H28B(0.045) H28C(0.045) H16A(0.036)
 H16B(0.036) H16C(0.036) H37(0.023) H40A(0.052) H40B(0.052) H40C(0.052)
 H25A(0.022) H25B(0.022) H32A(0.041) H32B(0.041) H32C(0.041) H10A(0.023)
 H10B(0.023) H26A(0.025) H26B(0.025) H21A(0.027) H21B(0.027) H29A(0.022)
 H29B(0.022) H34A(0.031) H34B(0.031) H38A(0.052) H38B(0.052) H38C(0.052)
 H42A(0.046) H42B(0.046) H42C(0.046) H18A(0.023) H18B(0.023) H39A(0.056)
 H39B(0.056) H39C(0.056) H41(0.03) H8A(0.042) H8B(0.042) H8C(0.042) H7A(0.028)
 H7B(0.028) H22A(0.032) H22B(0.032) H19A(0.033) H19B(0.033) H20A(0.053)
 H20B(0.053) H20C(0.053) H23A(0.044) H23B(0.044) H35A(0.033) H35B(0.033)
 H12A(0.072) H12B(0.072) H12C(0.072) H44(0.044) H11A(0.037) H11B(0.037)
 H36A(0.049) H36B(0.049) H36C(0.049) H24A(0.081) H24B(0.081) H24C(0.081)
 H43A(0.073) H43B(0.073) H43C(0.073) H45A(0.13) H45B(0.13) H45C(0.13)
 H28D(0.115) H28E(0.115)
 Fixed X: H4(0.8536) H3(1.0929) H29C(0.8912) H29D(0.8174) H6(0.8558)
 H5(1.0496) H2A(0.9574) H2B(0.8524) H14A(1.5958) H14B(1.6451) H13A(1.455)
 H13B(1.5017) H6A(1.4191) H6B(1.5321) H5A(1.5637) H5B(1.4592) H15A(1.4296)
 H15B(1.4816) H1A(0.8557) H1B(0.9628) H30A(1.396) H30B(1.5065) H31A(1.4635)
 H31B(1.5751) H27A(1.487) H27B(1.5336) H33A(1.2283) H33B(1.3045) H3A(1.1325)
 H3B(1.1318) H17A(1.6902) H17B(1.6765) H9A(1.6616) H9B(1.7392) H28A(1.4123)
 H28B(1.4913) H28C(1.3687) H16A(1.6148) H16B(1.4956) H16C(1.5631) H37(1.1102)
 H40A(0.7487) H40B(0.836) H40C(0.8705) H25A(1.4555) H25B(1.4843) H32A(1.6087)
 H32B(1.5976) H32C(1.4986) H10A(1.7083) H10B(1.7771) H26A(1.316) H26B(1.3517)
 H21A(1.2274) H21B(1.2333) H29A(1.3575) H29B(1.4665) H34A(1.2008) H34B(1.1121)
 H38A(1.1658) H38B(1.1241) H38C(1.2477) H42A(0.9373) H42B(0.9025) H42C(0.8139)
 H18A(1.5069) H18B(1.5022) H39A(1.117) H39B(1.2021) H39C(1.0751) H41(0.879)
 H8A(1.4164) H8B(1.3302) H8C(1.3057) H7A(1.3638) H7B(1.4742) H22A(1.3864)
 H22B(1.4006) H19A(1.6497) H19B(1.6618) H20A(1.4773) H20B(1.5686) H20C(1.488)
 H23A(1.2191) H23B(1.2353) H35A(1.1815) H35B(1.1166) H12A(1.7774) H12B(1.7981)
 H12C(1.896) H44(1.0292) H11A(1.9022) H11B(1.9) H36A(0.9606) H36B(1.0011)
 H36C(1.0247) H24A(1.2893) H24B(1.379) H24C(1.3902) H43A(1.1574) H43B(1.2751)
 H43C(1.2131) H45A(1.1742) H45B(1.2279) H45C(1.285) H28D(0.6308) H28E(0.5345)
 Fixed Y: H4(0.898) H3(0.5976) H29C(0.8699) H29D(0.8288) H6(0.6922) H5(0.7141)
 H2A(1.0143) H2B(1.0043) H14A(0.3138) H14B(0.2321) H13A(0.4358) H13B(0.3541)
 H6A(0.4914) H6B(0.4617) H5A(0.5753) H5B(0.5856) H15A(0.2965) H15B(0.2123)
 H1A(0.8208) H1B(0.7159) H30A(1.0207) H30B(1.002) H31A(0.8294) H31B(0.8131)
 H27A(1.2658) H27B(1.172) H33A(1.2261) H33B(1.17) H3A(0.7315) H3B(0.8457)
 H17A(0.4058) H17B(0.5102) H9A(0.322) H9B(0.299) H28A(1.2913) H28B(1.3368)
 H28C(1.385) H16A(0.0905) H16B(0.1194) H16C(0.1747) H37(0.436) H40A(0.667)
 H40B(0.7023) H40C(0.6109) H25A(1.1299) H25B(1.0479) H32A(0.8988) H32B(0.7951)
 H32C(0.9114) H10A(0.4553) H10B(0.4448) H26A(1.2644) H26B(1.1819) H21A(1.0278)
 H21B(1.1222) H29A(0.9309) H29B(0.9147) H34A(1.0611) H34B(1.1563) H38A(0.5467)
 H38B(0.4852) H38C(0.4301) H42A(0.4228) H42B(0.4023) H42C(0.4496) H18A(0.5061)
 H18B(0.611) H39A(0.3036) H39B(0.274) H39C(0.3429) H41(0.5304) H8A(0.557)
 H8B(0.6803) H8C(0.5914) H7A(0.6793) H7B(0.646) H22A(0.9006) H22B(0.9936)
 H19A(0.599) H19B(0.49) H20A(0.695) H20B(0.633) H20C(0.5861) H23A(0.9478)
 H23B(1.0388) H35A(1.1747) H35B(1.2791) H12A(0.312) H12B(0.2146) H12C(0.2135)
 H44(0.9403) H11A(0.3483) H11B(0.2628) H36A(1.2545) H36B(1.2424) H36C(1.1384)
 H24A(0.8842) H24B(0.8159) H24C(0.9082) H43A(0.9994) H43B(0.9004) H43C(0.9702)
 H45A(0.7338) H45B(0.7967) H45C(0.7305) H28D(0.8575) H28E(0.9273)
 Fixed Z: H4(0.3228) H3(0.1733) H29C(0.4146) H29D(0.4057) H6(0.3255)
 H5(0.3645) H2A(0.104) H2B(0.0826) H14A(0.3759) H14B(0.3214) H13A(0.3071)
 H13B(0.2529) H6A(0.1758) H6B(0.1411) H5A(0.2123) H5B(0.25) H15A(0.3711)
 H15B(0.3183) H1A(0.0826) H1B(0.1044) H30A(0.3485) H30B(0.3142) H31A(0.3625)
 H31B(0.3307) H27A(0.1595) H27B(0.112) H33A(0.2354) H33B(0.2947) H3A(0.1382)
 H3B(0.1354) H17A(0.3441) H17B(0.3042) H9A(0.1995) H9B(0.2583) H28A(0.033)
 H28B(0.0568) H28C(0.0805) H16A(0.3915) H16B(0.4167) H16C(0.4443) H37(0.1165)
 H40A(0.5466) H40B(0.5184) H40C(0.573) H25A(0.2275) H25B(0.1738) H32A(0.4146)
 H32B(0.4399) H32C(0.4468) H10A(0.158) H10B(0.2193) H26A(0.1617) H26B(0.1074)
 H21A(0.1885) H21B(0.1464) H29A(0.2683) H29B(0.2338) H34A(0.3052) H34B(0.2622)
 H38A(-0.0192) H38B(-0.0635) H38C(-0.0403) H42A(0.5425) H42B(0.476)
 H42C(0.5293) H18A(0.3823) H18B(0.3462) H39A(0.0593) H39B(0.0036) H39C(-0.0106)
 H41(0.3992) H8A(0.039) H8B(0.0401) H8C(0.0765) H7A(0.1486) H7B(0.1108)
 H22A(0.1423) H22B(0.103) H19A(0.4079) H19B(0.4419) H20A(0.4564) H20B(0.5086)
 H20C(0.4898) H23A(0.0871) H23B(0.0472) H35A(0.3846) H35B(0.34) H12A(0.0817)
 H12B(0.1306) H12C(0.0894) H44(0.4251) H11A(0.1438) H11B(0.1954) H36A(0.3439)
 H36B(0.4143) H36C(0.3777) H24A(-0.0104) H24B(0.0416) H24C(0) H43A(0.4395)
 H43B(0.4496) H43C(0.507) H45A(0.5299) H45B(0.5638) H45C(0.5044) H28D(0.0516)
 H28E(0.0185)
;