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_7032594
_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 unk
_chemical_formula_moiety         'C5 H12 Cr Mo6 O24, 3(C16 H36 N), 11(H2 O)'
_chemical_formula_sum            'C53 H142 Cr Mo6 N3 O35'
_chemical_formula_weight         2009.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   15.1562(5)
_cell_length_b                   21.7956(13)
_cell_length_c                   25.0114(13)
_cell_measurement_reflns_used    16230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.722
_cell_measurement_theta_min      0.599
_cell_volume                     8262.2(7)
_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      100(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28860
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.7361
_exptl_absorpt_correction_T_min  0.6122
_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    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4148
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         15854
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0305P)^2^+17.6685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                13981
_reflns_number_total             15854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound2b
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_database_code               7032594
_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, All O(H,H) groups
2. Restrained distances
 H6-HW1D
 2 with sigma of 0.02
 HW1B-HW7A
 2 with sigma of 0.02
 HW4B-HW1E
 2 with sigma of 0.01
 HW4B-HW1F
 3 with sigma of 0.01
 HW1C-HW8B
 2 with sigma of 0.02
 HW1C-HW8A
 2 with sigma of 0.02
 HW6A-HW8A
 2 with sigma of 0.02
 HW6B-HW9B
 2 with sigma of 0.02
 HW6B-HW7B
 2 with sigma of 0.02
 HW1C-H31F
 2 with sigma of 0.02
 HW6A-HW9B
 2.5 with sigma of 0.02
 HW3B-HW1E
 2 with sigma of 0.02
 C335-C333
 1.53 with sigma of 0.01
 H6-HW1C
 2 with sigma of 0.01
 HW1A-HW3A
 3 with sigma of 0.01
 HW3B-HW1F
 2 with sigma of 0.02
 HW3A-HW1F
 2 with sigma of 0.02
 HW6A-HW8B
 2 with sigma of 0.02
 HW2A-HW3A
 3 with sigma of 0.01
 HW4A-HW1C
 2 with sigma of 0.02
 HW4A-HW1D
 2 with sigma of 0.02
 H4-HW4A
 3 with sigma of 0.001
 H4-HW4B
 3 with sigma of 0.01
 HW1B-HW3B
 2 with sigma of 0.02
 HW1B-HW3A
 2 with sigma of 0.02
 H12A-HW8A
 2 with sigma of 0.02
 HW5B-HW1C
 2 with sigma of 0.02
 HW6A-HW9A
 2 with sigma of 0.02
 HW6B-HW7B
 2 with sigma of 0.02
 HW8B-HW1D
 2 with sigma of 0.02
 C335-C333
 1.53 with sigma of 0.02
 N1-C131 = N1-C121 = N1-C141 = N1-C111
 1.48 with sigma of 0.02
 N2-C221 = N2-C231 = N2-C241 = N2-C211
 1.48 with sigma of 0.02
 C252-C241
 1.53 with sigma of 0.02
 N3-C311 = N3-C331 = N3-C341 = N3-C321
 1.48 with sigma of 0.02
 C252-C241 = C253-C252 = C243-C242 = C244-C243 = C254-C253
 1.53 with sigma of 0.01
 C335-C333 = C313-C312 = C312-C311 = C353-C342 = C343-C342 = C344-C343 = C354-
 C353
 1.53 with sigma of 0.01
3. Rigid bond restraints
 C241, C242, C243, C244, C252, C253, C254
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C331, C332, C333, C335
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C341, C342, C343, C344, C353, C354
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C241 \\sim C242 \\sim C243 \\sim C244 \\sim C252 \\sim C253 \\sim C254: within
1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
C331 \\sim C332 \\sim C333 \\sim C335: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.01
C341 \\sim C342 \\sim C343 \\sim C344 \\sim C353 \\sim C354: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(OW11) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(OW3) \\sim Ueq, Uanis(OW1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(H24C)=Sof(H24D)=Sof(C242)=Sof(H24E)=Sof(H24F)=Sof(C243)=Sof(H24G)=
 Sof(H24H)=Sof(C244)=Sof(H24I)=Sof(H24J)=Sof(H24K)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C252)=Sof(H25A)=Sof(H25B)=Sof(C253)=Sof(H25C)=
 Sof(H25D)=Sof(C254)=Sof(H25E)=Sof(H25F)=Sof(H25G)=FVAR(1)
 Sof(H34E)=Sof(H34F)=Sof(C343)=Sof(H34G)=Sof(H34H)=Sof(C344)=Sof(H34I)=
 Sof(H34J)=Sof(H34K)=1-FVAR(2)
 Sof(H34C)=Sof(H34D)=Sof(C353)=Sof(H35A)=Sof(H35B)=Sof(C354)=Sof(H35C)=
 Sof(H35D)=Sof(H35E)=FVAR(2)
6.a Free rotating group:
 OW1(HW1A,HW1B), OW2(HW2A,HW2B), OW3(HW3A,HW3B), OW4(HW4A,HW4B), OW5(HW5A,
 HW5B), OW6(HW6A,HW6B), OW7(HW7A,HW7B), OW8(HW8A,HW8B), OW9(HW9A,HW9B),
 OW10(HW1C,HW1D), OW11(HW1E,HW1F)
6.b Ternary CH refined with riding coordinates:
 O4(H4), O5(H5), O6(H6)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C111(H11A,H11B), C112(H11C,H11D),
 C113(H11E,H11F), C121(H12A,H12B), C122(H12C,H12D), C123(H12E,H12F), C131(H13A,
 H13B), C132(H13C,H13D), C133(H13E,H13F), C141(H14A,H14B), C142(H14C,H14D),
 C143(H14E,H14F), C211(H21A,H21B), C212(H21C,H21D), C213(H21E,H21F), C221(H22A,
 H22B), C222(H22C,H22D), C223(H22E,H22F), C231(H23A,H23B), C232(H23C,H23D),
 C233(H23E,H23F), C241(H24C,H24D), C241(H24A,H24B), C242(H24E,H24F), C243(H24G,
 H24H), C252(H25A,H25B), C253(H25C,H25D), C311(H31A,H31B), C312(H31C,H31D),
 C313(H31E,H31F), C321(H32A,H32B), C322(H32C,H32D), C323(H32E,H32F), C331(H33A,
 H33B), C332(H33C,H33D), C333(H33E,H33F), C341(H34A,H34B), C342(H34E,H34F),
 C342(H34C,H34D), C343(H34G,H34H), C353(H35A,H35B)
6.d Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C114(H11G,H11H,H11I), C124(H12G,H12H,H12I), C134(H13G,H13H,
 H13I), C144(H14G,H14H,H14I), C214(H21G,H21H,H21I), C224(H22G,H22H,H22I),
 C234(H23G,H23H,H23I), C244(H24I,H24J,H24K), C254(H25E,H25F,H25G), C314(H31G,
 H31H,H31I), C324(H32G,H32H,H32I), C335(H33G,H33H,H33I), C344(H34I,H34J,H34K),
 C354(H35C,H35D,H35E)
;