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_7113305
_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         'C156 H258 Cu6 N42, 24(F6 P1), 26(C2 H3 N1)'
_chemical_formula_sum            'C208 H336 Cu6 F144 N68 P24'
_chemical_formula_weight         7649.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.8441(2)
_cell_length_b                   31.8441(2)
_cell_length_c                   31.8441(2)
_cell_measurement_reflns_used    6040
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.3047
_cell_measurement_theta_min      3.9231
_cell_volume                     32291.4(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -36.00   20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676   37.0000 -180.0000 56

  2 omega   75.00  139.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   23.0000  -68.0000 64

  3 omega -116.00  -18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676  -37.0000    0.0000 98

  4 omega -118.00   -9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676  -77.0000  150.0000 109
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0148830000
_diffrn_orient_matrix_UB_12      0.0441690000
_diffrn_orient_matrix_UB_13      -0.0129573000
_diffrn_orient_matrix_UB_21      0.0446505000
_diffrn_orient_matrix_UB_22      0.0171582000
_diffrn_orient_matrix_UB_23      0.0071808000
_diffrn_orient_matrix_UB_31      0.0111534000
_diffrn_orient_matrix_UB_32      -0.0097506000
_diffrn_orient_matrix_UB_33      -0.0460645000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13856
_diffrn_reflns_theta_full        66.919
_diffrn_reflns_theta_max         66.919
_diffrn_reflns_theta_min         3.926
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71348
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             15560
_exptl_crystal_size_max          0.1756
_exptl_crystal_size_mid          0.1478
_exptl_crystal_size_min          0.0357
_refine_diff_density_max         1.501
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1474
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.872
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.1338
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3689
_refine_ls_wR_factor_ref         0.3827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1213
_reflns_number_total             1474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49663e2.cif
_cod_data_source_block           Struct_2
_cod_original_cell_volume        32291.5(7)
_cod_database_code               7113305
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Restrained distances
 F6A-P2A
 1.6 with sigma of 0.02
 F6B-P2A
 1.6 with sigma of 0.02
 F5B-P2A
 1.6 with sigma of 0.02
 N4-C11
 1.15 with sigma of 0.02
 C12-C11
 1.54 with sigma of 0.02
 C3A-C4A
 1.54 with sigma of 0.02
 N1B-C3B
 1.15 with sigma of 0.02
 C3B-C4B
 1.54 with sigma of 0.02
 N3-C9A
 1.15 with sigma of 0.02
 N3-C9B
 1.15 with sigma of 0.02
 C10A-C9A
 1.54 with sigma of 0.02
 C10B-C9B
 1.54 with sigma of 0.02
 F6A-F4B
 2.115 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
F6A \\sim P2A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
F4A \\sim F4B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F3A \\sim F3B: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
N4 \\sim C11 \\sim C12: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N1B \\sim C3B \\sim C4B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C9A \\sim C10A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C9B \\sim C10B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F6A) \\sim Ueq, Uanis(F5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F6B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4B) \\sim Ueq, Uanis(F4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1B) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4B)
\\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C9B) \\sim Ueq, Uanis(C10B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(F4B)=0.5*(1-FVAR(2))
 Sof(F4A)=0.5*FVAR(2)
 Fixed Sof: P2A(0.1875) P2B(0.0625) F3A(0.43333) F3B(0.23333) F5A(0.0625)
 F6A(0.02083) F6B(0.25) F7A(0.16667) N1A(0.25) N1B(0.25) N2(0.25) N4(0.25)
 C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3A(0.25) H3AA(0.25)
 H3AB(0.25) C3B(0.25) C4A(0.25) H4AA(0.25) H4AB(0.25) C4B(0.25) H(0.25)
 HA(0.25) HB(0.25) C5(0.25) H5A(0.25) H5B(0.25) C6(0.25) C7(0.25) C8(0.25)
 HC(0.25) HD(0.25) HE(0.25) C9A(0.02083) C9B(0.10417) C10A(0.02083) HF(0.02083)
 HG(0.02083) HH(0.02083) C10B(0.10417) HI(0.10417) HJ(0.10417) HK(0.10417)
 C12(0.25) HL(0.25) HM(0.25) HN(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5(H5A,H5B)
5.b Me refined with riding coordinates:
 C4B(H,HA,HB), C8(HC,HD,HE), C10A(HF,HG,HH), C10B(HI,HJ,HK), C12(HL,HM,HN)
;
_smtbx_masks_special_details
;
Olex2 solvent masking procedure was used to remove electron density
corresponding to 16 PF6- anions and (estimated) 56 MeCN solvent molecules
in the unit cell (4 PF6- and 14 MeCN/formula unit). The omitted atoms are 
included in the formula and calculations.
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'