Step-by-Step Strategy from Achiral Precursors to Polyoxometalates-Based Chiral Organic-Inorganic Hybrids.
Zhang, Jiangwei; Luo, Jianhui; Wang, Pingmei; Ding, Bin; Huang, Yichao; Zhao, Zhenlin; Zhang, Jin; Wei, Yongge; Inorganic chemistry 54 (2015) 2551–2559; doi:10.1021/ic502622k

data_4342631
_publ_section_title
;
 Step-by-Step Strategy from Achiral Precursors to Polyoxometalates-Based
 Chiral Organic-Inorganic Hybrids.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2551
_journal_page_last               2559
_journal_paper_doi               10.1021/ic502622k
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C4 H11 Cr Mo6 N O24, Br, 4(C16 H36 N), 2(H2 O)'
_chemical_formula_sum            'C68 H162 Br Cr Mo6 N5 O26'
_chemical_formula_weight         2173.54
_chemical_name_systematic
;
 ? 
;
_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             2014-12-19
_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                 92.867(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3140(13)
_cell_length_b                   15.3614(6)
_cell_length_c                   18.1903(8)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      29.2382
_cell_measurement_theta_min      3.1546
_cell_volume                     4552.9(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      101(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega    8.00   47.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000  150.0000 39

  2 omega   27.00   90.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000   60.0000 63

  3 omega    0.00   83.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518   37.0000  -90.0000 83

  4 omega  -46.00   35.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       21.4518  -77.0000  -30.0000 81

  5 omega  -20.00    6.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -      -15.8268  -77.0000   60.0000 26

  6 omega  -77.00  -51.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -      -15.8268  -77.0000   60.0000 26

  7 omega  -51.00  -24.00   1.0000    2.3800
omega____ theta____ kappa____ phi______ frames
    -       20.9831  -37.0000  -60.0000 27
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0249018000
_diffrn_orient_matrix_UB_12      0.0378356000
_diffrn_orient_matrix_UB_13      -0.0025541000
_diffrn_orient_matrix_UB_21      0.0060300000
_diffrn_orient_matrix_UB_22      0.0023458000
_diffrn_orient_matrix_UB_23      -0.0383158000
_diffrn_orient_matrix_UB_31      -0.0351763000
_diffrn_orient_matrix_UB_32      -0.0263678000
_diffrn_orient_matrix_UB_33      -0.0071032000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28285
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.444
_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    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2233.4
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         17883
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0495P)^2^+6.0826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                13647
_reflns_number_total             17883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502622k_si_002.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 4342631--4342637.cif.'
_cod_original_cell_volume        4552.9(4)
_cod_database_code               4342631
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.02
 H1A-H1B
 1.55 with sigma of 0.02
 C7-H1A
 1.679 with sigma of 0.02
 C7-H1B
 2.164 with sigma of 0.02
 C62-H63B
 2 with sigma of 0.02
 C63-H62A
 2 with sigma of 0.02
 N4-C37 = N4-C49
 1.47 with sigma of 0.01
 C48A-C47
 1.53 with sigma of 0.01
 C44-C43
 1.53 with sigma of 0.01
 C66-C65 = C67-C66 = C68-C67
 1.53 with sigma of 0.01
 C68-C67
 1.5 with sigma of 0.01
 C23-H22A
 2 with sigma of 0.02
 C22-H23A
 2.067 with sigma of 0.02
 C24-H23A
 2.05 with sigma of 0.02
 C24-H23B
 1.844 with sigma of 0.02
 C23-H24A
 1.844 with sigma of 0.02
 C23-H24C
 2 with sigma of 0.02
 H1AD-H23A
 2 with sigma of 0.02
 C27-C26 = C27-C28
 1.53 with sigma of 0.01
 C1C-C18 = C1B-C17 = C20-C19
 1.53 with sigma of 0.01
 C31-C30 = C24-C23 = C36B-C35B = C36A-C35A = C35B-C34 = C34-C33
 1.53 with sigma of 0.01
 C48B-C47 = C48A-C47 = C52-C51 = C40-C39
 1.53 with sigma of 0.01
 C66-C65 = C60-C59 = C56-C55 = C54-C53
 1.53 with sigma of 0.01
 H67A-H26D
 2 with sigma of 0.02
 H67A-H26C
 2 with sigma of 0.02
 H67B-H26D
 2.2 with sigma of 0.01
 H67A-H26D
 2.2 with sigma of 0.01
 H26C-H67A
 2.2 with sigma of 0.01
 H26C-H67B
 2.2 with sigma of 0.01
 H26D-H65B
 2.2 with sigma of 0.01
 H26D-H67B
 2.2 with sigma of 0.01
 H20A-H68B
 2.2 with sigma of 0.01
 H26D-H67A
 3 with sigma of 0.01
3. Restrained angles
 H47D-C47-H47B
 fixed at 23 with sigma of 0.02
 C62-C63-H63B
 fixed at 108 with sigma of 0.02
 C63-C62-H62B
 fixed at 108 with sigma of 0.02
 C62-C63-H63B
 fixed at 109 with sigma of 0.02
 C67-C68-H68B
 fixed at 107 with sigma of 0.02
 C59-C60-H60B
 fixed at 110 with sigma of 0.02
 C59-C60-H60C
 fixed at 110 with sigma of 0.02
 C59-C60-H60A
 fixed at 110 with sigma of 0.02
 C67-C68-H68C
 fixed at 109 with sigma of 0.02
4. Rigid bond restraints
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C47, C48A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C67: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C67 \\sim C66 \\sim C65: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C26 \\sim C25: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C25 \\sim C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C48B) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C35B) \\sim Ueq,
Uanis(C48B) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C36A) \\sim Ueq,
Uanis(C36B) \\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C67) = Uanis(C68)
6. Others
 Sof(H34C)=Sof(H34D)=1-FVAR(1)
 Sof(H34A)=Sof(H34B)=FVAR(1)
 Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(2)
 Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=FVAR(2)
 Sof(O26A)=Sof(H26C)=Sof(H26D)=FVAR(3)
 Fixed Sof: C35B(0.5) H35A(0.5) H35B(0.5) C36B(0.5) H36A(0.5) H36B(0.5)
 H36C(0.5) C35A(0.5) H35C(0.5) H35D(0.5) C36A(0.5) H36D(0.5) H36E(0.5) H36F(0.5)
7.a Free rotating group:
 O26A(H26C,H26D), O1A(H1AC,H1AD)
7.b Ternary CH refined with riding coordinates:
 O5(H5), O6(H6), O4(H4)
7.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C1(H1C,H1D), C49(H49A,H49B), C45(H45A,H45B),
 C17(H17A,H17B), C41(H41A,H41B), C8(H8A,H8B), C50(H50A,H50B), C9(H9A,H9B),
 C10(H10A,H10B), C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C14(H14A,H14B),
  C13(H13A,H13B), C31(H31A,H31B), C51(H51A,H51B), C37(H37A,H37B), C46(H46A,
 H46B), C42(H42A,H42B), C34(H34C,H34D), C34(H34A,H34B), C29(H29A,H29B),
 C15(H15A,H15B), C19(H19A,H19B), C16(H16A,H16B), C22(H22A,H22B), C18(H18A,H18B),
  C25(H25A,H25B), C33(H33A,H33B), C21(H21A,H21B), C26(H26A,H26B), C23(H23A,
 H23B), C47(H47C,H47D), C47(H47A,H47B), C1A(H1AA,H1AB), C30(H30A,H30B),
 C1B(H1BA,H1BB), C35B(H35A,H35B), C61(H61A,H61B), C63(H63A,H63B), C53(H53A,
 H53B), C62(H62A,H62B), C57(H57A,H57B), C54(H54A,H54B), C65(H65A,H65B),
 C55(H55A,H55B), C66(H66A,H66B), C59(H59A,H59B), C67(H67A,H67B), C35A(H35C,
 H35D), C58(H58A,H58B), C27(H27A,H27B)
7.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C40(H40A,H40B,H40C), C11(H11A,H11B,H11C), C32(H32A,H32B,
 H32C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C1C(H1CA,H1CB,H1CC), C64(H64A,
 H64B,H64C), C48B(H48A,H48B,H48C), C36B(H36A,H36B,H36C), C56(H56A,H56B,H56C),
 C20(H20A,H20B,H20C), C60(H60A,H60B,H60C), C24(H24A,H24B,H24C), C36A(H36D,H36E,
 H36F), C48A(H48D,H48E,H48F), C28(H28A,H28B,H28C), C68(H68A,H68B,H68C)
;