Sterically controlled self-assembly of tetrahedral M6L4 cages via cationic N-donor ligands
Anssi Peuronen; Samu Forsblom; Manu Lahtinen; Chem.Commun. 50 (2014) 5469–; doi:10.1039/C3CC49663E

data_7113306
_publ_section_title
;
 Sterically controlled self-assembly of tetrahedral M6L4 cages via
 cationic N-donor ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              5469
_journal_paper_doi               10.1039/C3CC49663E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'C144 H252 Cu6 N36 O6, 12(C1 O3 F3 S1), 12(C2 N1 O4 F6 S2) 5(C2 H3 N1)'
_chemical_formula_sum            'C190 H267 Cu6 F108 N53 O90 S36'
_chemical_formula_weight         8320.95
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.2831(2)
_cell_length_b                   25.2831(2)
_cell_length_c                   25.2831(2)
_cell_measurement_reflns_used    1822
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      62.1344
_cell_measurement_theta_min      4.2798
_cell_volume                     16161.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega  -74.00  -38.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7071   77.0000 -180.0000 36

  2 omega   12.00   81.00   1.0000  250.0000
omega____ theta____ kappa____ phi______ frames
    -       84.1918  -30.0000  -30.0000 69
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0038144000
_diffrn_orient_matrix_UB_12      0.0296214000
_diffrn_orient_matrix_UB_13      -0.0531214000
_diffrn_orient_matrix_UB_21      -0.0069660000
_diffrn_orient_matrix_UB_22      0.0526678000
_diffrn_orient_matrix_UB_23      0.0298679000
_diffrn_orient_matrix_UB_31      0.0603967000
_diffrn_orient_matrix_UB_32      0.0078819000
_diffrn_orient_matrix_UB_33      0.0000993000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5126
_diffrn_reflns_theta_full        62.224
_diffrn_reflns_theta_max         62.224
_diffrn_reflns_theta_min         4.283
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.951
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             8440
_exptl_crystal_size_max          0.1472
_exptl_crystal_size_mid          0.1144
_exptl_crystal_size_min          0.0502
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 475 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1233P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.506
_reflns_Friedel_fraction_full    0.506
_reflns_Friedel_fraction_max     0.579
_reflns_number_gt                1485
_reflns_number_total             1889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49663e2.cif
_cod_data_source_block           Struct_3
_cod_original_cell_volume        16161.8(4)
_cod_database_code               7113306
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N3-C9
 1.15 with sigma of 0.01
 C9-C10
 1.54 with sigma of 0.01
 O1-H1
 0.85 with sigma of 0.01
 H1-H1_$1
 1.387 with sigma of 0.02
3. Restrained planarity
 F1, H1, O1, Cu1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N3 \\sim C9 \\sim C10: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
F1 \\sim C11 \\sim S1 \\sim O2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.006
Uanis(O1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.006
5. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H4A(0.5) H4B(0.5) H5A(0.5) H5B(0.5) H8A(0.5)
 H8B(0.5) H8C(0.5) H10A(0.5) H10B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
6.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_smtbx_masks_special_details
;
Olex2 solvent masking procedure was used to remove electron density
corresponding to 16 OTf- and 24 Ntf2- anions and (estimated) 10 MeCN
solvent molecules in the unit cell (8 PF6-, 12 Ntf2- and 5 MeCN/formula
unit). The omitted atoms are included in the formula and calculations.
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'