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_7032591
_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         'C4 H12 Cr Mo6 N O24, 2(C4 H12 N O3), 6(H2 O)'
_chemical_formula_sum            'C12 H48 Cr Mo6 N3 O36'
_chemical_formula_weight         1438.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.022(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9934(3)
_cell_length_b                   11.6341(4)
_cell_length_c                   22.8845(6)
_cell_measurement_reflns_used    8830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.9978
_cell_measurement_theta_min      29.2259
_cell_volume                     3952.79(19)
_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 0.998
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20213
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.224
_exptl_absorpt_correction_T_max  0.8599
_exptl_absorpt_correction_T_min  0.7315
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         7777
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0226P)^2^+5.7310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                6710
_reflns_number_total             7777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound1a
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        3952.77(19)
_cod_database_code               7032591
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H4 of O4, H5 of O5, H6 of O6, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups, H29A of O29A, H29B of O29B, H28 of O28, H27 of O27, H26
  of O26, H25 of O25, H30A of O30A, H30B of O30B
2. Restrained distances
 H6-HW2B = HW1A-H29B
 -2.2 with sigma of 0.01
 OW1-HW1A = OW1-HW1B = OW2-HW2A = OW2-HW2B = OW3-HW3A = OW3-HW3B
 0.84 with sigma of 0.02
 OW4-HW4A = OW4-HW4B = OW5-HW5A = OW5-HW5B = OW6-HW6A = OW6-HW6B
 0.84 with sigma of 0.02
 OW1-HW1A = OW2-HW2B
 0.82 with sigma of 0.02
 N1-C4
 1.46 with sigma of 0.02
 HW1A-HW1B = HW2A-HW2B = HW3A-HW3B = HW4A-HW4B = HW5A-HW5B = HW6A-HW6B
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C11B)
Uanis(O29A) = Uanis(O29B)
Uanis(C12A) = Uanis(C12B)
Uanis(O30A) = Uanis(O30B)
4. Same fragment restrains
{C10, O28}
as
{C11B, O29B}
{C10, O28}
as
{C11A, O29A}
{C10, O28}
as
{C12A, O30A}
{C10, O28}
as
{C12B, O30B}
5. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(O29A)=Sof(H29A)=Sof(C12B)=Sof(H12C)=
 Sof(H12D)=Sof(O30B)=Sof(H30B)=1-FVAR(1)
 Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(O29B)=Sof(H29B)=Sof(C12A)=Sof(H12A)=
 Sof(H12B)=Sof(O30A)=Sof(H30A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 O4(H4), O5(H5), O6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C10(H10A,H10B), C11B(H11A,H11B), C11A(H11C,H11D), C12A(H12A,H12B), C12B(H12C,
 H12D)
6.c Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E)
6.d Idealised tetrahedral OH refined as rotating group:
 O25(H25), O26(H26), O27(H27), O28(H28), O29B(H29B), O29A(H29A), O30A(H30A),
 O30B(H30B)
;