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_7032596
_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         'C6 H14 Cr Mo6 O24, 4(C16 H36 N),H4 N'
_chemical_formula_sum            'C70 H162 Br2 Cr Mo6 N5 O24'
_chemical_formula_weight         2245.43
_chemical_name_systematic
;
 ? 
;
_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 Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.7125(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5994(3)
_cell_length_b                   26.2375(6)
_cell_length_c                   22.1200(4)
_cell_measurement_reflns_used    18942
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      0.415
_cell_measurement_theta_min      0.362
_cell_volume                     9629.5(3)
_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      103(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42577
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         18882
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4563.25
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         18882
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0435P)^2^+24.0061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1086
_reflns_number_gt                14367
_reflns_number_total             18882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound3b
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        9629.6(3)
_cod_database_code               7032596
_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,H,H) groups
 At 1.5 times of:
  All O(H) groups, {H13G,H13H,H13I} of C134, {H14G,H14H,H14I} of C144, {H21G,
  H21H,H21I} of C214, {H22G,H22H,H22I} of C224, {H23G,H23H,H23I} of C234, {H24G,
  H24H,H24I} of C244, {H31G,H31H,H31I} of C314, {H32G,H32H,H32I} of C324, {H33G,
  H33H,H33I} of C334, {H34M,H34N,H34O} of C344, {H34P,H34Q,H34R} of C345, {H41G,
  H41H,H41I} of C414, {H42G,H42H,H42I} of C424, {H6A,H6B,H6C} of C6, {H11G,H11H,
  H11I} of C114, {H12G,H12H,H12I} of C124, {H44G,H44H,H44I} of C444
 At 1.1 times of:
  {H43G,H43H,H43I} of C434
2. Restrained distances
 N3-C341 = N3-C311 = N3-C321 = N3-C331
 1.47 with sigma of 0.02
 C341-C340 = C343-C342 = C343-C340 = C345-C343 = C344-C343
 1.53 with sigma of 0.02
 C345-C343 = C344-C343
 1.55 with sigma of 0.01
 N3-C341 = N3-C311 = N3-C331 = N3-C321
 1.47 with sigma of 0.01
 C244-C243
 1.53 with sigma of 0.02
 N2-C231 = N2-C221 = N2-C211 = N2-C241
 1.47 with sigma of 0.02
 C144-C143 = C143-C142
 1.53 with sigma of 0.02
 C143-C142 = C144-C143
 1.53 with sigma of 0.01
 C433-C432 = C434-C433
 1.53 with sigma of 0.02
 C433-C432 = C434-C433
 1.53 with sigma of 0.01
 C345-C343 = C344-C343
 1.56 with sigma of 0.01
 N5-H5C \\sim N5-H5D \\sim N5-H5E \\sim N5-H5F
 with sigma of 0.02
3. Rigid bond restraints
 C142, C143
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C341, C340, C342, C343, C344, C345
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C142 \\sim C143: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C434 \\sim C433: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C143) \\sim Ueq, Uanis(C345) \\sim Ueq, Uanis(C434) \\sim Ueq,
Uanis(C340) \\sim Ueq, Uanis(C342) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: H34A(0.5) H34B(0.5) H34C(0.5) H34D(0.5) C340(0.5) H34E(0.5)
 H34F(0.5) C342(0.5) H34G(0.5) H34H(0.5) H34I(0.5) H34J(0.5) H34K(0.5)
 H34L(0.5) C344(0.5) H34M(0.5) H34N(0.5) H34O(0.5) C345(0.5) H34P(0.5)
 H34Q(0.5) H34R(0.5)
6.a Ternary CH refined with riding coordinates:
 O4(H4), O5(H5), O6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), 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(H24A,H24B), C242(H24C,H24D), C243(H24E,
 H24F), 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), C341(H34C,H34D), C340(H34E,H34F), C342(H34G,H34H),
 C343(H34I,H34J), C343(H34K,H34L), C411(H41A,H41B), C412(H41C,H41D), C413(H41E,
 H41F), C421(H42A,H42B), C422(H42C,H42D), C423(H42E,H42F), C431(H43A,H43B),
 C432(H43C,H43D), C433(H43E,H43F), C441(H44A,H44B), C442(H44C,H44D), C443(H44E,
 H44F)
6.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), 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(H24G,H24H,H24I), C314(H31G,H31H,H31I), C324(H32G,
 H32H,H32I), C334(H33G,H33H,H33I), C344(H34M,H34N,H34O), C345(H34P,H34Q,H34R),
 C414(H41G,H41H,H41I), C424(H42G,H42H,H42I), C434(H43G,H43H,H43I), C444(H44G,
 H44H,H44I)
;