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_7032593
_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_formula_moiety
'C5 H12 Cr Mo6 O24 3-, 3(C16 H36 N 1+), 3(H2 O)'
_chemical_formula_sum            'C53 H126 Cr Mo6 N3 O27'
_chemical_formula_weight         1865.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2004(17)
_cell_length_b                   23.3540(14)
_cell_length_c                   15.3020(16)
_cell_measurement_reflns_used    1252
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.05
_cell_volume                     9005.7(12)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5864
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_platon_squeeze_details
;
;
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         9068
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0547
_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^+370.5782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                9043
_reflns_number_total             9068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        9005.7(13)
_cod_database_code               7032593
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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
 C11-H11B
 0.9 with sigma of 0.02
 C29-C25
 2.5 with sigma of 0.02
 N1-C21
 1.5 with sigma of 0.02
 C29-C21
 2.5 with sigma of 0.02
 C25-C26
 1.53 with sigma of 0.02
 C31-C32
 1.53 with sigma of 0.02
 C26-C27
 1.53 with sigma of 0.02
 C27-C28
 1.53 with sigma of 0.02
 C31-C29
 2.5 with sigma of 0.02
 C32-C30
 2.5 with sigma of 0.02
 C32-C30
 2.5 with sigma of 0.02
 C29-C30
 1.53 with sigma of 0.02
 C21-C25
 2.5 with sigma of 0.02
 C30-C31
 1.53 with sigma of 0.02
 C25-C27
 2.5 with sigma of 0.02
 H11B-H1AC
 2 with sigma of 0.02
 C24-C23
 1.5 with sigma of 0.02
 N1-C25 = N1-C21 = N1-C29
 1.47 with sigma of 0.01
 C22-C21 = C23-C22 = C24-C23
 1.53 with sigma of 0.01
 N2-C13 = N2-C7
 1.47 with sigma of 0.01
 N2-C17
 1.45 with sigma of 0.01
 C11-C8 = C1A-C11 = C20-C19 = C1B-C12 = C12-C10
 1.53 with sigma of 0.02
 C16-C15
 1.53 with sigma of 0.01
 C9-C10
 1.53 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(C14) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C17)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O12) \\sim
Ueq, Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C28) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O14) \\sim Ueq,
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1B) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O8)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.0001 and
sigma for terminal atoms of 0.0002
Uanis(C23) = Uanis(C24)
Uanis(C21) = Uanis(N1) = Uanis(C29)
Uanis(C1B) = Uanis(C12)
Uanis(C18) = Uanis(C19) = Uanis(C20)
4. Others
 Fixed Sof: H1(0.25) H3A(0.5) H3B(0.5) H6A(0.5) H6B(0.5) H6C(0.5) H25A(0.5)
 H25B(0.5) H30A(0.5) H30B(0.5) H29A(0.5) H29B(0.5) H31A(0.5) H31B(0.5)
 H16D(0.5) H16E(0.25) H17C(0.5) H17D(0.5) H26A(0.5) H26B(0.5) C28(0.5)
 H28A(0.5) H28B(0.5) H28C(0.5) H32A(0.5) H32B(0.5) H32C(0.5)
5.a Free rotating group:
 O15(H15C,H15D), O16(H16D,H16E), O17(H17C,H17D)
5.b Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), C27(H27)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C17(H17A,H17B), C13(H13A,H13B),
 C18(H18A,H18B), C9(H9A,H9B), C8(H8A,H8B), C14(H14A,H14B), C15(H15A,H15B),
 C10(H10A,H10B), C19(H19A,H19B), C25(H25A,H25B), C12(H12A,H12B), C30(H30A,H30B),
  C29(H29A,H29B), C31(H31A,H31B), C21(H21A,H21B), C26(H26A,H26B), C23(H23A,
 H23B), C22(H22A,H22B)
5.d Aromatic/amide H refined with riding coordinates:
 C11(H11A)
5.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C1A(H1AA,H1AB,
 H1AC), C1B(H1BA,H1BB,H1BC), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C), C32(H32A,
 H32B,H32C)
;