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_7032595
_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         'C5 H12 Cr Mo6 O24, Br,4(C16 H36 N)'
_chemical_formula_sum            'C69 H156 Br Cr Mo6 N4 O24'
_chemical_formula_weight         2133.52
_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                 92.631(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1276(6)
_cell_length_b                   15.4530(4)
_cell_length_c                   18.2045(3)
_cell_measurement_reflns_used    17803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.752
_cell_measurement_theta_min      0.571
_cell_volume                     4532.1(2)
_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  'SHELXL-97 (Sheldrick, 1997)'
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39453
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         39453
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_correction_T_min  0.5992
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         17739
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0654P)^2^+21.1323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                15827
_reflns_number_total             17739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound2c
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        4532.2(2)
_cod_database_code               7032595
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61B-C60B
 1.53 with sigma of 0.02
 C69-C68
 1.53 with sigma of 0.02
 C1-C5
 1.53 with sigma of 0.02
 C5-C1
 1.5 with sigma of 0.02
 N2-C26 = N2-C34 = N2-C30
 1.47 with sigma of 0.02
 C29B-C28 = C28-C27 = C33-C32 = C37B-C36 = C25-C24 = C23-C22
 1.53 with sigma of 0.02
 C45B-C44B = C44B-C43
 1.53 with sigma of 0.01
 C52B-C51 = C53A-C52B
 1.53 with sigma of 0.01
 C47-C46 = C48-C47 = C49-C48 = C39-C38 = C40-C39
 1.53 with sigma of 0.01
 N4-C66B = N4-C62A = N4-C58B = N4-C54B
 1.47 with sigma of 0.01
 C56-C55 = C57-C56 = C63-C62A = C64-C63 = C65-C64 = C67B-C66B = C68-C67B = C69-
 C68
 1.53 with sigma of 0.01
 N1-C7 = N1-C18 = N1-C10
 1.47 with sigma of 0.01
 C11-C10 = C12-C8 = C21-C20
 1.53 with sigma of 0.01
 N2-C34 = N2-C30 = N2-C26
 1.47 with sigma of 0.01
 C28-C27 = C29B-C28 = C27-C26 = C25-C24 = C37B-C36 = C33-C32 = C23-C22 = C24-C23
 1.53 with sigma of 0.01
 H40B-H57B
 2 with sigma of 0.02
 C57-H57A
 0.95 with sigma of 0.02
 C57-H57B
 0.95 with sigma of 0.02
 C57-H57C
 0.95 with sigma of 0.02
3. Rigid bond restraints
 N4, C66B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim C1 \\sim C3 \\sim C6 \\sim C2: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C61B \\sim C60B \\sim C59 \\sim C58B \\sim C54B \\sim C55 \\sim C56 \\sim C57
\\sim C66B \\sim C67B \\sim C68 \\sim C69 \\sim C63 \\sim C64 \\sim C65: within
1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N4 \\sim N3 \\sim N2 \\sim N1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C52B \\sim C51: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C66B \\sim C54B \\sim C58B \\sim C68 \\sim C69 \\sim C48 \\sim C49: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C5 \\sim C2 \\sim C1 \\sim C6 \\sim C3: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.08
C5 \\sim C1 \\sim C2 \\sim C3 \\sim C6: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C5) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C45B) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C63)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C41B) \\sim Ueq, Uanis(C41A) \\sim Ueq, Uanis(C52B) \\sim Ueq,
Uanis(C53A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C66B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) = Uanis(N3) = Uanis(N1) = Uanis(N2)
Uanis(C69) = Uanis(C68)
Uanis(C60B) = Uanis(C61B)
Uanis(C63) = Uanis(C64)
Uanis(C64) = Uanis(C65)
Uanis(C6) = Uanis(C2) = Uanis(C5) = Uanis(C1) = Uanis(C3)
Uanis(C51) = Uanis(C43)
Uanis(C41A) = Uanis(C41B)
5. Others
 Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=FVAR(1)
 Sof(H36A)=Sof(H36B)=1-FVAR(2)
 Sof(H43A)=Sof(H43B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=1-FVAR(3)
6.a Ternary CH refined with riding coordinates:
 O4(H4), O6(H6), O5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C31(H31A,H31B), C32(H32A,H32B),
 C26(H26A,H26B), C30(H30A,H30B), C22(H22A,H22B), C34(H34A,H34B), C7(H7A,H7B),
 C8(H8A,H8B), C14(H14A,H14B), C27(H27A,H27B), C23(H23A,H23B), C9(H9A,H9B),
 C18(H18A,H18B), C11(H11A,H11B), C19(H19A,H19B), C20(H20A,H20B), C16(H16A,H16B),
  C35(H35A,H35B), C10(H10A,H10B), C42(H42A,H42B), C39(H39A,H39B), C38(H38A,
 H38B), C15(H15A,H15B), C36(H36A,H36B), C24(H24A,H24B), C17(H17A,H17B),
 C46(H46A,H46B), C47(H47A,H47B), C43(H43A,H43B), C28(H28A,H28B), C48(H48A,H48B),
  C50(H50A,H50B), C51(H51A,H51B), C40(H40C,H40D), C40(H40A,H40B), C52B(H52A,
 H52B), C55(H55A,H55B), C60B(H60A,H60B), C56(H56A,H56B), C58B(H58A,H58B),
 C59(H59A,H59B), C54B(H54A,H54B), C44B(H44A,H44B), C66B(H66A,H66B), C64(H64A,
 H64B), C63(H63A,H63B), C68(H68A,H68B), C67B(H67A,H67B), C62A(H62A,H62B)
6.c Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C12(H12A,H12B,H12C), C37B(H37A,H37B,
 H37C), C13(H13A,H13B,H13C), C1A(H1AA,H1AB,H1AC), C29B(H29A,H29B,H29C),
 C61B(H61A,H61B,H61C), C21(H21A,H21B,H21C), C45B(H45A,H45B,H45C), C49(H49A,H49B,
 H49C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C)
6.d Idealised Me refined as rotating group:
 C41B(H41A,H41B,H41C), C57(H57A,H57B,H57C), C25(H25A,H25B,H25C), C41A(H41D,
 H41E,H41F), C53A(H53A,H53B,H53C)
;