Spontaneous resolution of polyoxometalate-based inorganic-organic hybrids driven by solvent and common ion.
Zhang, Jiangwei; Zhao, Zhenlin; Zhang, Jin; She, Shan; Huang, Yichao; Wei, Yongge; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17296–17302; doi:10.1039/c4dt01954g

data_7032592
_publ_section_title
;
 Spontaneous resolution of polyoxometalate-based inorganic-organic hybrids
 driven by solvent and common ion.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17296
_journal_page_last               17302
_journal_paper_doi               10.1039/c4dt01954g
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C4 H11 Cr Mo6 N O24 3-, Br 1-, 4(C16 H36 N 1+), 2(H2 O)'
_chemical_formula_sum            'C68 H162 Br Cr Mo6 N5 O26'
_chemical_formula_weight         2173.54
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.867(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3140(13)
_cell_length_b                   15.3614(6)
_cell_length_c                   18.1903(8)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      29.2382
_cell_measurement_theta_min      3.1546
_cell_volume                     4552.9(5)
_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      101(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    8.00   47.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000  150.0000 39

  2 omega   27.00   90.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000   60.0000 63

  3 omega    0.00   83.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000  -90.0000 83

  4 omega  -46.00   35.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518  -77.0000  -30.0000 81

  5 omega  -20.00    6.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -      -15.8268  -77.0000   60.0000 26

  6 omega  -77.00  -51.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -      -15.8268  -77.0000   60.0000 26

  7 omega  -51.00  -24.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       20.9831  -37.0000  -60.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0249018000
_diffrn_orient_matrix_UB_12      0.0378356000
_diffrn_orient_matrix_UB_13      -0.0025541000
_diffrn_orient_matrix_UB_21      0.0060300000
_diffrn_orient_matrix_UB_22      0.0023458000
_diffrn_orient_matrix_UB_23      -0.0383158000
_diffrn_orient_matrix_UB_31      -0.0351763000
_diffrn_orient_matrix_UB_32      -0.0263678000
_diffrn_orient_matrix_UB_33      -0.0071032000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28285
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.444
_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    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2233.4
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         17883
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0495P)^2^+6.0826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                13647
_reflns_number_total             17883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound1b
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        4552.9(4)
_cod_database_code               7032592
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.02
 H1A-H1B
 1.55 with sigma of 0.02
 C7-H1A
 1.679 with sigma of 0.02
 C7-H1B
 2.164 with sigma of 0.02
 C62-H63B
 2 with sigma of 0.02
 C63-H62A
 2 with sigma of 0.02
 N4-C37 = N4-C49
 1.47 with sigma of 0.01
 C48A-C47
 1.53 with sigma of 0.01
 C44-C43
 1.53 with sigma of 0.01
 C66-C65 = C67-C66 = C68-C67
 1.53 with sigma of 0.01
 C68-C67
 1.5 with sigma of 0.01
 C23-H22A
 2 with sigma of 0.02
 C22-H23A
 2.067 with sigma of 0.02
 C24-H23A
 2.05 with sigma of 0.02
 C24-H23B
 1.844 with sigma of 0.02
 C23-H24A
 1.844 with sigma of 0.02
 C23-H24C
 2 with sigma of 0.02
 H1AD-H23A
 2 with sigma of 0.02
 C48A-H48D
 0.96 with sigma of 0.02
 C48A-H48F
 0.96 with sigma of 0.02
 C27-C26 = C27-C28
 1.53 with sigma of 0.01
 C1C-C18 = C1B-C17 = C20-C19
 1.53 with sigma of 0.01
 C31-C30 = C24-C23 = C36B-C35B = C36A-C35A = C35B-C34 = C34-C33
 1.53 with sigma of 0.01
 C48B-C47 = C48A-C47 = C52-C51 = C40-C39
 1.53 with sigma of 0.01
 C66-C65 = C60-C59 = C56-C55 = C54-C53
 1.53 with sigma of 0.01
 H67A-H26D
 2 with sigma of 0.02
 H67A-H26C
 2 with sigma of 0.02
 C48A-H48E
 0.95 with sigma of 0.02
3. Restrained angles
 H47D-C47-H47B
 fixed at 23 with sigma of 0.02
 H47A-C47-H48E
 fixed at 110 with sigma of 0.02
 C47-C48A-H48E
 fixed at 110 with sigma of 0.02
 C47-C48A-H48F
 fixed at 110 with sigma of 0.02
 C47-C48A-H48D
 fixed at 109 with sigma of 0.02
 C47-C48A-H48E
 fixed at 109 with sigma of 0.02
 C62-C63-H63B
 fixed at 108 with sigma of 0.02
 C63-C62-H62B
 fixed at 108 with sigma of 0.02
 C62-C63-H63B
 fixed at 109 with sigma of 0.02
 C67-C68-H68B
 fixed at 107 with sigma of 0.02
 C59-C60-H60B
 fixed at 110 with sigma of 0.02
 C59-C60-H60C
 fixed at 110 with sigma of 0.02
 C59-C60-H60A
 fixed at 110 with sigma of 0.02
 C67-C68-H68C
 fixed at 109 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C67: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C67 \\sim C66 \\sim C65: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C26 \\sim C25: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C25 \\sim C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(H34A)=Sof(H34B)=FVAR(1)
 Sof(H47C)=Sof(H47D)=Sof(C48B)=1-FVAR(2)
 Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=FVAR(2)
 Sof(O26A)=Sof(H26C)=Sof(H26D)=FVAR(3)
 Fixed Sof: C35B(0.5) H35A(0.5) H35B(0.5) C36B(0.5) H36A(0.5) H36B(0.5)
 H36C(0.5) C35A(0.5) H35C(0.5) H35D(0.5) C36A(0.5) H36D(0.5) H36E(0.5) H36F(0.5)
6.a Free rotating group:
 O26A(H26C,H26D), O1A(H1AC,H1AD)
6.b Ternary CH refined with riding coordinates:
 O5(H5), O6(H6), O4(H4)
6.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C1(H1C,H1D), C49(H49A,H49B), C45(H45A,H45B),
 C17(H17A,H17B), C41(H41A,H41B), C8(H8A,H8B), C50(H50A,H50B), C9(H9A,H9B),
 C10(H10A,H10B), C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C14(H14A,H14B),
  C13(H13A,H13B), C31(H31A,H31B), C51(H51A,H51B), C37(H37A,H37B), C46(H46A,
 H46B), C42(H42A,H42B), C34(H34C,H34D), C34(H34A,H34B), C29(H29A,H29B),
 C15(H15A,H15B), C19(H19A,H19B), C16(H16A,H16B), C22(H22A,H22B), C18(H18A,H18B),
  C25(H25A,H25B), C33(H33A,H33B), C21(H21A,H21B), C26(H26A,H26B), C23(H23A,
 H23B), C47(H47C,H47D), C47(H47A,H47B), C1A(H1AA,H1AB), C30(H30A,H30B),
 C1B(H1BA,H1BB), C35B(H35A,H35B), C61(H61A,H61B), C63(H63A,H63B), C53(H53A,
 H53B), C62(H62A,H62B), C57(H57A,H57B), C54(H54A,H54B), C65(H65A,H65B),
 C55(H55A,H55B), C66(H66A,H66B), C59(H59A,H59B), C67(H67A,H67B), C35A(H35C,
 H35D), C58(H58A,H58B), C27(H27A,H27B)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C40(H40A,H40B,H40C), C11(H11A,H11B,H11C), C32(H32A,H32B,
 H32C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C1C(H1CA,H1CB,H1CC), C64(H64A,
 H64B,H64C), C48B(H48A,H48B,H48C), C36B(H36A,H36B,H36C), C56(H56A,H56B,H56C),
 C20(H20A,H20B,H20C), C60(H60A,H60B,H60C), C24(H24A,H24B,H24C), C36A(H36D,H36E,
 H36F), C48A(H48D,H48E,H48F), C28(H28A,H28B,H28C), C68(H68A,H68B,H68C)
;