Reversible transformation between chiral and achiral Dy6Mo4 clusters through a symmetric operation
Yong Zheng; Yin-Yin Pan; Yan-Ping Ren; La-Sheng Long; Rong-Bin Huang; Lan-Sun Zheng; Chem.Commun. 50 (2014) 14728–; doi:10.1039/C4cc07047J

data_7115996
_publ_section_title
;
 Reversible transformation between chiral and achiral Dy6Mo4 clusters
 through a symmetric operation
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_journal_name_full               Chem.Commun.
_journal_page_first              14728
_journal_paper_doi               10.1039/C4cc07047J
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H64 Dy6 Mo4 N4 O40, 2(C4 H12 N)'
_chemical_formula_sum            'C65 H120 Dy6 Mo4 N6 O55'
_chemical_formula_weight         3224.43
_chemical_name_systematic
;
 ? 
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_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.9826(6)
_cell_length_b                   21.9826(6)
_cell_length_c                   19.1459(7)
_cell_measurement_temperature    153(2)
_cell_volume                     8012.4(4)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.1244
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20432
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.685
_exptl_absorpt_correction_T_max  0.7056
_exptl_absorpt_correction_T_min  0.2559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4668
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.724
_refine_diff_density_rms         0.252
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10486
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.1015
_refine_ls_shift/su_max          0.154
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+177.2512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2257
_reflns_number_gt                8291
_reflns_number_total             10486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07047j2.cif
_cod_data_source_block           complex_IIIb
_cod_database_code               7115996
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C27
 1.6 with sigma of 0.02
 C25-C26
 1.6 with sigma of 0.02
 N3-C29
 1.8 with sigma of 0.02
 C26-O17
 2.3 with sigma of 0.02
 O18-C25
 1.2 with sigma of 0.02
 O17-C25
 1.2 with sigma of 0.02
 C27-O20
 1.25 with sigma of 0.02
 C30-C32
 2.4 with sigma of 0.02
 N3-C31
 1.8 with sigma of 0.02
 N3-C31
 1.5 with sigma of 0.02
3. Restrained planarity
 C26, C25, O18, O17
 with sigma of 0.1
4. Rigid bond restraints
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C8 \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C16 \\sim C17: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C26) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
6.a Ternary CH refined with riding coordinates:
 C9(H9), C19(H19)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C18(H18A,H18B), C20(H20A,H20B)
6.c Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C15(H15), C14(H14),
 C13(H13), C17(H17)
6.e Fitted hexagon refined as free rotating group:
 C12(C11,C16,C15,C14,C13)
6.f Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
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