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_7115993
_publ_section_title
;
 Reversible transformation between chiral and achiral Dy6Mo4 clusters
 through a symmetric operation
;
_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(C6 H16 N)'
_chemical_formula_sum            'C68 H132 Dy6 Mo4 N6 O58'
_chemical_formula_weight         3320.55
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2013-04-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr  9 2013 14:06:00, GUI svn.r4458)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.9687(2)
_cell_length_b                   21.9687(2)
_cell_length_c                   19.0989(3)
_cell_measurement_temperature    133(2)
_cell_volume                     7982.66(16)
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.992
_diffrn_reflns_theta_min         2.826
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  0.2568
_exptl_absorpt_correction_T_min  0.2193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis RED'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_description       block
_exptl_crystal_F_000             4830
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.537
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         10454
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+8.1328P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9516
_reflns_number_total             10454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07047j2.cif
_cod_data_source_block           complex_IIa
_cod_original_cell_volume        7982.66(19)
_cod_database_code               7115993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C31 = C31-C33
 2.5 with sigma of 0.02
 N3-C29 = N3-C31 = N3-C33
 1.46 with sigma of 0.02
 C29-C30 = C31-C32 = C33-C34
 1.54 with sigma of 0.02
 N3-C32 = N3-C34
 2.55 with sigma of 0.02
3. Rigid bond restraints
 C1, C6
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.01
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O15 \\sim C23: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.005
N3 \\sim C33 \\sim C31 \\sim C32 \\sim N3 \\sim C29 \\sim C33 \\sim C34: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(N3) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C9(H9), C19(H19), N3(H3a)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C10(H10a,H10b), C18(H18a,H18b), C20(H20a,H20b), C33(H33a,H33b),
 C29(H29a,H29b), C31(H31a,H31b)
5.c Me refined with riding coordinates:
 C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C28(H28a,H28b,H28c), C30(H30a,H30b,
 H30c), C34(H34a,H34b,H34c), C32(H32a,H32b,H32c)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17)
5.e Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c)
;
_shelx_estimated_absorpt_t_max   0.332
_shelx_estimated_absorpt_t_min   0.290
_shelx_res_checksum              61780
_shelxl_version_number           2013-2