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_7115995
_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 H62 Gd6 Mo4 N4 O40, 2(C4 H12 N)'
_chemical_formula_sum            'C65 H120 Gd6 Mo4 N6 O55'
_chemical_formula_weight         3192.93
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.761(3)
_cell_length_b                   21.761(3)
_cell_length_c                   19.354(4)
_cell_measurement_temperature    173(2)
_cell_volume                     7937(2)
_computing_cell_refinement       RAPID
_computing_data_collection       R-AXIS-SPIDER
_computing_data_reduction        RAPID
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-CS Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10380
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.253
_exptl_absorpt_correction_T_max  0.6757
_exptl_absorpt_correction_T_min  0.5679
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa_analytical
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10380
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.196
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+12.5936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                5726
_reflns_number_total             10380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07047j2.cif
_cod_data_source_block           complex_IIIa
_cod_database_code               7115995
_olex2_refinement_description
;
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
 C23-C24 = C21-C22 = C27-C28
 1.25 with sigma of 0.02
 N3-C29
 1.6 with sigma of 0.02
 N3-C32
 1.6 with sigma of 0.02
3. Restrained planarity
 C23, C24, O15, O16
 with sigma of 0.1
4. Rigid bond restraints
 O20, C27, C3, C4, C4, C5, C27, C28
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.001
 O13, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O14, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O16, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C8 \\sim C9: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.001
O1 \\sim C1 \\sim C2 \\sim C1 \\sim C6 \\sim C7: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.001
O15 \\sim C23 \\sim C1 \\sim C6 \\sim C27 \\sim C28: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.001
C23 \\sim C24: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.001
Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.001
Uanis(C24) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C28) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.001
Uanis(O13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C29) \\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:
 C10(H10A,H10B), C18(H18A,H18B), C20(H20A,H20B)
6.c Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17)
6.e Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C)
;