Self-Assembly of Water-Mediated Supramolecular Cationic Archimedean Solids
Peuronen, Anssi; Lehtimäki, Esa; Lahtinen, Manu; Crystal Growth & Design 13 (2013) 4615–; doi:10.1021/cg401246n

data_4508352
_publ_section_title
;
 Self-Assembly of Water-Mediated Supramolecular Cationic Archimedean
 Solids
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4615
_journal_paper_doi               10.1021/cg401246n
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety
'4(F24 K1 P4), 4(F6 P1), 12(H O0.5), 4(C30 H51 N6)'
_chemical_formula_sum            'C120 H216 F120 K4 N24 O6 P20'
_chemical_formula_weight         5146.97
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_symmetry_space_group_name_Hall  'P -4 2 3'
_symmetry_space_group_name_H-M   'P -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   17.73792(17)
_cell_length_b                   17.73792(17)
_cell_length_c                   17.73792(17)
_cell_measurement_reflns_used    2780
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.4091
_cell_measurement_theta_min      3.5209
_cell_volume                     5580.95(9)
_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
;
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
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -61.00  -14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -77.0000   60.0000 47

  2 omega   56.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -120.0000 40

  3 omega   39.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 37
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0457090000
_diffrn_orient_matrix_UB_12      -0.0543952000
_diffrn_orient_matrix_UB_13      -0.0500381000
_diffrn_orient_matrix_UB_21      -0.0536665000
_diffrn_orient_matrix_UB_22      -0.0156954000
_diffrn_orient_matrix_UB_23      0.0665109000
_diffrn_orient_matrix_UB_31      -0.0504238000
_diffrn_orient_matrix_UB_32      0.0660378000
_diffrn_orient_matrix_UB_33      -0.0249818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4296
_diffrn_reflns_theta_full        66.61
_diffrn_reflns_theta_max         76.61
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.438
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_correction_T_min  0.578
_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            colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.2435
_exptl_crystal_size_mid          0.1833
_exptl_crystal_size_min          0.1594
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         1723
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1072P)^2^+3.5187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                1633
_reflns_number_total             1723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401246n_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4508352
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
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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 F(H) groups
2. Restrained distances
 H1-O1
 0.85 with sigma of 0.01
 F7B-P2B
 1.55 with sigma of 0.02
 H1-H1_$1
 1.347 with sigma of 0.02
3. Restrained planarity
 N1, H1, O1, H1_$1, N1_$2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C3 \\sim N1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F6B \\sim F7B \\sim F4B \\sim F6B \\sim F5B: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
P2B \\sim P2A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
K2B \\sim K2A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F7B) \\sim Ueq, Uanis(F7A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(K2B) \\sim Ueq, Uanis(K2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(P2B)=Sof(F4B)=Sof(F7B)=0.5*(1-FVAR(2))
 Sof(K2B)=0.125*(1-FVAR(2))
 Sof(K2A)=0.125*FVAR(2)
 Sof(P2A)=Sof(F3A)=Sof(F4A)=Sof(F6A)=Sof(F7A)=0.5*FVAR(2)
 Sof(F5A)=FVAR(1)
 Fixed Sof: F8(0.08333) F9(0.33333) F10(0.08333) 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)
 Fixed Z: K2A(-0.48131) K2B(-0.49917)
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 Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
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