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_4508350
_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         'F24 K P4, C27 H45 N6'
_chemical_formula_sum            'C27 H45 F24 K N6 P4'
_chemical_formula_weight         1072.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9664(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.7662(2)
_cell_length_b                   16.8462(3)
_cell_length_c                   8.50641(11)
_cell_measurement_reflns_used    5114
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.8990
_cell_measurement_theta_min      4.1490
_cell_volume                     1962.02(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -111.00  -10.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -77.0000  -90.0000 101

  2 omega  -48.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426   37.0000 -120.0000 80

  3 omega -113.00  -88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.5000 -111.0000 -150.0000 25

  4 omega   44.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 47

  5 omega   38.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000 -180.0000 92

  6 omega   89.00  155.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   60.0000 66

  7 omega   36.00   88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 52

  8 omega   54.00  155.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000 -150.0000 101

  9 omega   47.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   90.0000 36

 10 omega -118.00   -9.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -77.0000  120.0000 109

 11 omega   23.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7426 -125.0000   60.0000 75

 12 omega   39.00   99.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 60

 13 omega   36.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 80

 14 omega   59.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000  -60.0000 119
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0995319000
_diffrn_orient_matrix_UB_12      -0.0282910000
_diffrn_orient_matrix_UB_13      -0.0463800000
_diffrn_orient_matrix_UB_21      -0.0447869000
_diffrn_orient_matrix_UB_22      -0.0103059000
_diffrn_orient_matrix_UB_23      -0.1724333000
_diffrn_orient_matrix_UB_31      0.0272369000
_diffrn_orient_matrix_UB_32      0.0863485000
_diffrn_orient_matrix_UB_33      -0.0359130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5677
_diffrn_reflns_theta_full        66.95
_diffrn_reflns_theta_max         66.95
_diffrn_reflns_theta_min         4.16
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.2994
_exptl_crystal_size_mid          0.1994
_exptl_crystal_size_min          0.1757
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+3.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                3295
_reflns_number_total             3317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401246n_si_002.cif
_cod_data_source_block           1a
_cod_database_code               4508350
_olex2_refinement_description
;
1. Others
 Fixed Sof: H9A(0.5) H1(0.5) H10A(0.5) H2(0.5) H12A(0.5) H3(0.5)
 Fixed U12: K1(0) P2(0) P3(0) F7(0) F8(0) F10(0) F11(0) F13(0) F14(0) N3(0)
 N4(0) C9(0) C10(0) C12(0) C13(0) C16(0)
 Fixed U23: K1(0) P2(0) P3(0) F7(0) F8(0) F10(0) F11(0) F13(0) F14(0) N3(0)
 N4(0) C9(0) C10(0) C12(0) C13(0) C16(0)
 Fixed Uiso: H1A(0.04) H1B(0.04) H2A(0.026) H2B(0.026) H3A(0.032) H3B(0.032)
 H4A(0.026) H4B(0.026) H5A(0.032) H5B(0.032) H6A(0.027) H6B(0.027) H7A(0.065)
 H7B(0.065) H8A(0.031) H8B(0.031) H9A(0.044) H1(0.044) H10A(0.034) H2(0.034)
 H11A(0.023) H11B(0.023) H12A(0.024) H3(0.024) H13(0.02) H15(0.02)
 Fixed X: H1A(1.011) H1B(0.9694) H2A(0.8668) H2B(0.9123) H3A(1.1988)
 H3B(1.1452) H4A(1.0514) H4B(1.1017) H5A(1.0484) H5B(1.1377) H6A(1.0342)
 H6B(0.9444) H7A(0.641) H7B(0.7425) H8A(0.7551) H8B(0.6539) H9A(0.4924)
 H1(0.4924) H10A(0.4966) H2(0.4966) H11A(0.9423) H11B(0.8517) H12A(0.5991)
 H3(0.5991) H13(0.9705) H15(0.7485)
 Fixed Y: K1(0) P2(0) P3(0) F7(0) F8(0) F10(0) F11(0) F13(0) F14(0) N3(0.5)
 N4(0.5) H1A(0.749) H1B(0.8251) H2A(0.7475) H2B(0.6707) H3A(0.707) H3B(0.6763)
 H4A(0.5993) H4B(0.6333) H5A(0.8715) H5B(0.8221) H6A(0.7537) H6B(0.8003)
 H7A(0.6179) H7B(0.5712) H8A(0.5733) H8B(0.6214) C9(0.5) H9A(0.4525) H1(0.5475)
 C10(0.5) H10A(0.5476) H2(0.4524) H11A(0.635) H11B(0.6829) C12(0.5)
 H12A(0.5474) H3(0.4526) C13(0.5) H13(0.5) H15(0.6203) C16(0.5)
 Fixed Z: H1A(0.3051) H1B(0.3887) H2A(0.5001) H2B(0.4234) H3A(0.6002)
 H3B(0.4355) H4A(0.5658) H4B(0.731) H5A(0.6376) H5B(0.7249) H6A(0.8499)
 H6B(0.7563) H7A(-0.0324) H7B(-0.0257) H8A(0.2361) H8B(0.2293) H9A(-0.0465) H1(-
 0.0465) H10A(0.2128) H2(0.2128) H11A(0.8462) H11B(0.7608) H12A(0.4563)
 H3(0.4563) H13(0.781) H15(0.5379)
;