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_7032597
_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         'C6 H14 Cr Mo6 O24, Br, 4(C16 H36 N)'
_chemical_formula_sum            'C70 H158 Br Cr Mo6 N4 O24'
_chemical_formula_weight         2147.55
_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                 93.3530(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1185(3)
_cell_length_b                   15.6094(3)
_cell_length_c                   18.3046(3)
_cell_measurement_reflns_used    16530
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      72.64
_cell_measurement_theta_min      3.72
_cell_volume                     4597.56(14)
_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      104(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36622
_diffrn_reflns_theta_full        72.64
_diffrn_reflns_theta_max         72.64
_diffrn_reflns_theta_min         3.72
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.476
_exptl_absorpt_correction_T_max  0.184
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224.0
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         16530
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0542
_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^)+(0.1093P)^2^+28.4262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                15955
_reflns_number_total             16530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01954g2.cif
_cod_data_source_block           compound3c
_cod_depositor_comments
'Adding full bibliography for 7032591--7032597.cif.'
_cod_original_cell_volume        4597.55(16)
_cod_database_code               7032597
_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
 C25A-C26B
 1.53 with sigma of 0.02
 C33B-C32B
 1.53 with sigma of 0.02
 C12B-C10 = C22-C21 = C21-C20 = C9A-C8 = C9B-C8
 1.53 with sigma of 0.01
 C9A-C10A = C9B-C10B
 1.53 with sigma of 0.01
 C25A-C24 = C32B-C31B = C34B-C33B = C29-C30 = C29-C28B = C28B-C27 = C37A-C36A =
  C38A-C37A
 1.53 with sigma of 0.01
 C71-C70
 1.53 with sigma of 0.01
 C42-C41 = C41-C40
 1.53 with sigma of 0.01
 C31B-C33B
 2.5 with sigma of 0.01
 C36A-C35 = C33B-C32B
 1.53 with sigma of 0.01
 H10F-H22C
 2 with sigma of 0.02
 C30-H30A
 0.98 with sigma of 0.02
 C30-H30B
 0.98 with sigma of 0.02
 C30-H30C
 0.98 with sigma of 0.02
3. Rigid bond restraints
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25A, C26B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31B, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33B, C34B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C34B) \\sim Ueq, Uanis(C32B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C9A) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(C8) \\sim Ueq, Uanis(C26B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C10A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C28B) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(O11) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C31B) \\sim Ueq, Uanis(O4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C9B)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C32B) = Uanis(C33B)
5. Others
 Fixed Sof: H8BC(0.5) H8BD(0.5) H8AA(0.5) H8AB(0.5) C9B(0.5) H9BA(0.5)
 H9BB(0.5) C10B(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5)
 C10A(0.5) H10D(0.5) H10E(0.5) H10F(0.5)
6.a Ternary CH refined with riding coordinates:
 O4(H4), O6(H6), O5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C52(H52A,H52B), C2(H2A,H2B), C43(H43A,H43B), C1(H1A,
 H1B), C53(H53A,H53B), C45(H45A,H45B), C60(H60A,H60B), C39(H39A,H39B), C40(H40A,
 H40B), C44(H44A,H44B), C64(H64A,H64B), C48(H48A,H48B), C65(H65A,H65B),
 C56(H56A,H56B), C68(H68A,H68B), C61(H61A,H61B), C66(H66A,H66B), C57(H57A,H57B),
  C50(H50A,H50B), C49(H49A,H49B), C54(H54A,H54B), C69(H69A,H69B), C62(H62A,
 H62B), C58(H58A,H58B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C70(H70A,H70B), C7(H7A,H7B), C41(H41A,H41B), C19(H19A,H19B), C21(H21A,H21B),
 C20(H20A,H20B), C11(H11A,H11B), C8(H8BC,H8BD), C8(H8AA,H8AB), C24(H24A,H24B),
 C23(H23A,H23B), C27(H27A,H27B), C12B(H12A,H12B), C28B(H28A,H28B), C9B(H9BA,
 H9BB), C35(H35A,H35B), C32B(H32A,H32B), C31B(H31A,H31B), C33B(H33A,H33B),
 C9A(H9AA,H9AB), C36A(H36A,H36B), C37A(H37A,H37B), C29(H29A,H29B), C10(H10G,
 H10H), C25A(H25A,H25B)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C67(H67A,H67B,H67C), C55(H55A,H55B,H55C), C51(H51A,H51B,
 H51C), C63(H63A,H63B,H63C), C59(H59A,H59B,H59C), C42(H42A,H42B,H42C), C71(H71A,
 H71B,H71C), C18(H18A,H18B,H18C), C47(H47A,H47B,H47C), C13B(H13A,H13B,H13C),
 C10B(H10A,H10B,H10C), C22(H22A,H22B,H22C), C26B(H26A,H26B,H26C), C34B(H34A,
 H34B,H34C), C10A(H10D,H10E,H10F), C38A(H38A,H38B,H38C), C30(H30A,H30B,H30C)
;