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_7117202
_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 O24, Br, 3(C16 H36 N), C3 H7 N O,C2 H3 N, 2(C2 H6 O)'
_chemical_formula_sum            'C62 H143 Br Cr Mo6 N5 O27'
_chemical_formula_weight         2098.36
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.540(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0245(12)
_cell_length_b                   13.9963(6)
_cell_length_c                   26.7955(14)
_cell_measurement_reflns_used    12318
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2463
_cell_measurement_theta_min      3.0691
_cell_volume                     8981.8(8)
_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      100(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -56.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9711  -77.0000  -90.0000 59

  2 omega  -59.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9711  -77.0000 -150.0000 27

  3 omega  -85.00  -58.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9711  -37.0000  150.0000 27

  4 omega  -16.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273    0.0000 -180.0000 94

  5 omega  -50.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1273  -37.0000  150.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0278284000
_diffrn_orient_matrix_UB_12      0.0016453000
_diffrn_orient_matrix_UB_13      -0.0069658000
_diffrn_orient_matrix_UB_21      -0.0095943000
_diffrn_orient_matrix_UB_22      -0.0113448000
_diffrn_orient_matrix_UB_23      -0.0250094000
_diffrn_orient_matrix_UB_31      -0.0031151000
_diffrn_orient_matrix_UB_32      0.0493995000
_diffrn_orient_matrix_UB_33      -0.0055173000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47768
_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    1.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85692
_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    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3693
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.003
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         17618
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0391P)^2^+102.7294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                12347
_reflns_number_total             17618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        8981.8(7)
_cod_database_code               7117202
_audit_block_doi                 10.5517/cc146zgs
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1 of O1, H6 of O6, H4 of O4, H5 of O5, All C(H,H) groups,
  All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H1BA of O1B, H30 of O30
2. Restrained distances
 C48-C50
 2.5 with sigma of 0.02
 C17-C16
 1.53 with sigma of 0.01
 C7-C6
 1.53 with sigma of 0.01
 C28-C27
 1.53 with sigma of 0.01
 C25A-C23 = C25B-C23
 1.53 with sigma of 0.01
 C32B-C31 = C32A-C31
 1.53 with sigma of 0.01
 C33B-C32B = C34A-C33A = C34B-C33B
 1.53 with sigma of 0.01
 C42-C41
 1.53 with sigma of 0.01
 C41-C40 = C40-C39
 1.53 with sigma of 0.01
 C54B-C53 = C53-C51
 1.53 with sigma of 0.01
 C48-C47 = C49-C48 = C50-C49
 1.53 with sigma of 0.01
 C44B-C43 = C46B-C45B
 1.53 with sigma of 0.01
 C53-C51
 2.5 with sigma of 0.01
 C43-C45B
 2.5 with sigma of 0.01
 C44B-C46B
 2.5 with sigma of 0.01
 C44B-C45B
 1.53 with sigma of 0.01
 N3-C51
 1.47 with sigma of 0.01
 C52-C51
 1.53 with sigma of 0.01
 C51-C53
 2.5 with sigma of 0.01
 C54B-C52
 2.5 with sigma of 0.01
 H48B-H51A
 2 with sigma of 0.02
 H48B-H51A
 3 with sigma of 0.02
 H39A-H44B
 2 with sigma of 0.02
 H1EC-H34E
 2 with sigma of 0.02
 O30-C1D
 2.7 with sigma of 0.02
 C46B-C45B = C54B-C53 = C53-C52 = C45B-C44B
 1.53 with sigma of 0.01
 C51-C43
 2.6 with sigma of 0.01
 C39-C41
 2.5 with sigma of 0.01
 N3-C39
 1.47 with sigma of 0.01
 C54B-C53
 1.53 with sigma of 0.01
 C49-C47
 2.5 with sigma of 0.01
 C47-C39
 2.5 with sigma of 0.01
 N3-C40 = C43-C39
 2.5 with sigma of 0.01
3. Restrained dihedral angles
 O17-Mo3-O2-C1
 fixed at 179 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C42) \\sim Ueq, Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C53) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of
0.00001 and sigma for terminal atoms of 0.00002
Uanis(C48) = Uanis(C50) = Uanis(C49) = Uanis(C47)
Uanis(C51) = Uanis(N3)
Uanis(C40) = Uanis(C39)
5. Others
 Sof(H23C)=Sof(H23D)=Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C25B)=Sof(H25A)=
 Sof(H25B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C34B)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C33A)=Sof(H33C)=Sof(H33D)=Sof(C34A)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=FVAR(1)
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32A)=Sof(H32B)=1-FVAR(2)
 Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32C)=Sof(H32D)=FVAR(2)
 Fixed Uiso: C44B(0.3124) C52(0.3)
6.a Ternary CH refined with riding coordinates:
 O1(H1), O6(H6), O4(H4), O5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C19(H19A,H19B), C27(H27A,
 H27B), C18(H18A,H18B), C20(H20A,H20B), C7(H7A,H7B), C10(H10A,H10B), C31(H31C,
 H31D), C31(H31A,H31B), C15(H15A,H15B), C28(H28A,H28B), C14(H14A,H14B),
 C11(H11A,H11B), C36(H36A,H36B), C35(H35A,H35B), C8(H8A,H8B), C29(H29A,H29B),
 C23(H23C,H23D), C23(H23A,H23B), C22(H22A,H22B), C16(H16A,H16B), C37(H37A,H37B),
  C12(H12A,H12B), C32B(H32A,H32B), C33B(H33A,H33B), C25B(H25A,H25B), C48(H48A,
 H48B), C47(H47A,H47B), C43(H43A,H43B), C39(H39A,H39B), C49(H49A,H49B),
 C40(H40A,H40B), C41(H41A,H41B), C45B(H45A,H45B), C53(H53A,H53B), C44B(H44A,
 H44B), C51(H51A,H51B), C25A(H25C,H25D), C33A(H33C,H33D), C32A(H32C,H32D),
 C52(H52A,H52B), C1F(H1FA,H1FB), C1C(H1CA,H1CB)
6.c Aromatic/amide H refined with riding coordinates:
 C57(H57)
6.d Tetrahedral OH refined with riding coordinates:
 O30(H30), O1B(H1BA)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C38(H38A,H38B,H38C),
 C30(H30A,H30B,H30C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C26B(H26A,H26B,
 H26C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C34B(H34A,H34B,H34C),
 C42(H42A,H42B,H42C), C46B(H46A,H46B,H46C), C54B(H54A,H54B,H54C), C50(H50A,H50B,
 H50C), C1A(H1AA,H1AB,H1AC), C26A(H26D,H26E,H26F), C34A(H34D,H34E,H34F),
 C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,H1EC)
;