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_7113304
_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 H234 Cu6 N42, 24(F6 P), 32(C2 H3 N)'
_chemical_formula_sum            'C208 H330 Cu6 F144 N74 P24'
_chemical_formula_weight         7727.96
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           134
_space_group_name_Hall           '-P 4ac 2bc'
_space_group_name_H-M_alt        'P 42/n n m'
_symmetry_space_group_name_Hall  '-P 4ac 2bc'
_symmetry_space_group_name_H-M   'P 42/n n m :2'
_atom_sites_solution_hydrogens   geom
_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                   22.4999(5)
_cell_length_b                   22.4999(5)
_cell_length_c                   31.3098(12)
_cell_measurement_reflns_used    10342
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.7651
_cell_measurement_theta_min      3.1131
_cell_volume                     15850.4(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega -108.00  -79.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676 -155.0000  140.0000 29

  2 omega  -49.00   33.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676   37.0000 -180.0000 82

  3 omega   50.00   80.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000 -150.0000 30

  4 omega   43.00   75.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000  -30.0000 32

  5 omega   35.00   99.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -45.0000   30.0000 64

  6 omega   79.00  146.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -15.0000    0.0000 67

  7 omega -118.00   -9.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676  -77.0000   60.0000 109

  8 omega -115.00  -14.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676  -57.0000 -180.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0638019000
_diffrn_orient_matrix_UB_12      -0.0067384000
_diffrn_orient_matrix_UB_13      -0.0172644000
_diffrn_orient_matrix_UB_21      -0.0235487000
_diffrn_orient_matrix_UB_22      0.0382090000
_diffrn_orient_matrix_UB_23      0.0370696000
_diffrn_orient_matrix_UB_31      0.0083794000
_diffrn_orient_matrix_UB_32      0.0565026000
_diffrn_orient_matrix_UB_33      -0.0271991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1033
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            45580
_diffrn_reflns_theta_full        66.986
_diffrn_reflns_theta_max         66.986
_diffrn_reflns_theta_min         3.116
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.894
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.655
_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 light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       prism
_exptl_crystal_F_000             7852
_exptl_crystal_size_max          0.1531
_exptl_crystal_size_mid          0.0692
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0939
_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          0.2699
_refine_ls_wR_factor_ref         0.2989
_reflns_number_gt                4526
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49663e2.cif
_cod_data_source_block           Struct_1
_cod_original_cell_volume        15850.4(9)
_cod_database_code               7113304
_shelxl_version_number           2013-4
_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. Uiso/Uaniso restraints and constraints
Uanis(N8A) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4B) \\sim Ueq, Uanis(F3B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F9B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N8B) \\sim Ueq, Uanis(C23B) \\sim Ueq, Uanis(C24B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(F8B)=Sof(F9B)=1-FVAR(1)
 Sof(F8A)=Sof(F9A)=FVAR(1)
 Fixed Sof: N6(0.5) N8A(0.125) N8B(0.125) H9A(0.5) H9B(0.5) H10A(0.5)
 H10B(0.5) H12A(0.5) H12B(0.5) C19(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) C23A(0.125) C23B(0.125) C24A(0.125) H(0.125)
 HA(0.125) HB(0.125) C24B(0.125) HC(0.125) HD(0.125) HE(0.125) F3A(0.375)
 F3B(0.25) F4A(0.375) F4B(0.25) F5(0.375) H26A(0.5) H26B(0.5) H26C(0.5)
 F4C(0.375)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
4.b Me refined with riding coordinates:
 C24A(H,HA,HB), C24B(HC,HD,HE), C26(H26A,H26B,H26C)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C28(H28A,H28B,
 H28C)
;
_smtbx_masks_special_details
;
Olex2 solvent masking procedure was used to remove electron density
corresponding to 16 PF6- anions and (estimated) 40 MeCN solvent molecules in the 
unit cell (8 PF6- and 20 MeCN/formula unit). The masked PF6- anions could be 
identified from the electron density map but were too severely disordered for an
agreeable structure refinement. The  omitted atoms are included in the formula 
and calculations.
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'