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_4342633
_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 Mn Mo6 N O24, Br,  4(C16 H36 N)'
_chemical_formula_sum            'C68 H155 Br Mn Mo6 N5 O24'
_chemical_formula_weight         2137.45
_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 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.043(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1269(13)
_cell_length_b                   15.5347(6)
_cell_length_c                   17.9890(8)
_cell_measurement_reflns_used    28285
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.16
_cell_volume                     4500.4(5)
_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      293(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  0.0295
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29107
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2204.0
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         17288
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0426P)^2^+2.0404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                14104
_reflns_number_total             17288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502622k_si_002.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4342631--4342637.cif.'
_cod_original_cell_volume        4500.4(4)
_cod_database_code               4342633
_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
2. Restrained distances
 N1-H1A
 0.9 with sigma of 0.02
 H1A-H1B
 1.55 with sigma of 0.02
 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
 C4-H1A
 1.679 with sigma of 0.02
 C4-H1B
 2.164 with sigma of 0.02
 C62-H63B
 2 with sigma of 0.02
 C63-H62A
 2 with sigma of 0.02
 C16-C15 = C14-C13 = C18-C17 = C20-C19
 1.53 with sigma of 0.01
 C24-C23 = C22-C21 = C34-C33 = C35B-C34 = C36A-C35A = C36B-C35B = C31-C30 =
 C27B-C26 = C28B-C27B
 1.53 with sigma of 0.01
 C40-C39 = C52-C51 = C51-C50 = C50-C49 = C48A-C47 = C48B-C47
 1.53 with sigma of 0.02
 C68-C67 = C67-C66 = C66-C65 = C60-C59 = C59-C58 = C64-C63 = C63-C62 = C54-
 C53B = C55-C54 = C56-C55
 1.53 with sigma of 0.02
 C68-C67
 1.45 with sigma of 0.01
 C26-C21
 2.5 with sigma of 0.01
 N3-C26
 2.5 with sigma of 0.01
 C27B-C25
 2.5 with sigma of 0.01
 C28B-C26
 2.5 with sigma of 0.01
 N1-H1B
 0.8 with sigma of 0.01
 C67-C66 = C68-C67
 1.53 with sigma of 0.01
 C25-C21
 2.5 with sigma of 0.01
 C26-C25
 1.53 with sigma of 0.01
 C68-C66
 2.5 with sigma of 0.01
 H21B-H26A
 2.5 with sigma of 0.01
3. Rigid bond restraints
 C63, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27B, C28B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. 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
C28B \\sim C27B \\sim C26 \\sim C25: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C48B) \\sim Ueq, Uanis(C35B) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C36B)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C48A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(H34C)=Sof(H34D)=Sof(C35B)=Sof(H35A)=Sof(H35B)=1-FVAR(1)
 Sof(H34A)=Sof(H34B)=Sof(C35A)=Sof(H35C)=Sof(H35D)=FVAR(1)
 Sof(C36B)=Sof(H36A)=Sof(H36B)=Sof(H36C)=1-FVAR(2)
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=FVAR(2)
 Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=1-FVAR(3)
 Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 O5(H5), O6(H6), O4(H4)
6.b 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), C5(H5A,H5B), C50(H50A,H50B), C6(H6A,H6B),
 C7(H7A,H7B), 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), C11(H11A,
 H11B), C19(H19A,H19B), C9(H9A,H9B), C22(H22A,H22B), C15(H15A,H15B), C25(H25A,
 H25B), C33(H33A,H33B), C21(H21A,H21B), C26(H26A,H26B), C23(H23A,H23B),
 C47(H47C,H47D), C47(H47A,H47B), C10(H10A,H10B), C30(H30A,H30B), C18(H18A,H18B),
  C35B(H35A,H35B), C61(H61A,H61B), C27B(H27A,H27B), C63(H63A,H63B), C53B(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)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C40(H40A,H40B,H40C), C8(H8A,H8B,H8C), C32(H32A,H32B,
 H32C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C16(H16A,H16B,H16C), C64(H64A,
 H64B,H64C), C48B(H48A,H48B,H48C), C36B(H36A,H36B,H36C), C56(H56A,H56B,H56C),
 C20(H20A,H20B,H20C), C28B(H28A,H28B,H28C), C60(H60A,H60B,H60C), C24(H24A,H24B,
 H24C), C36A(H36D,H36E,H36F), C48A(H48D,H48E,H48F), C68(H68A,H68B,H68C)
;