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_4508353
_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_formula_moiety
'6(F6 P), 13(H2 O), H2 O0.63, 0.37(O), 2(C30 H51 N6)'
_chemical_formula_sum            'C60 H130 F36 N12 O14 P6'
_chemical_formula_weight         2113.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.8733(16)
_cell_angle_beta                 93.7874(16)
_cell_angle_gamma                90.4275(17)
_cell_formula_units_Z            2
_cell_length_a                   12.7737(3)
_cell_length_b                   14.4820(3)
_cell_length_c                   23.5105(4)
_cell_measurement_reflns_used    23615
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.3350
_cell_measurement_theta_min      3.4540
_cell_volume                     4339.02(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
SHELXL, 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -69.00   32.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   57.0000  120.0000 202

  2 omega  -70.00   32.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   57.0000 -120.0000 204

  3 omega  -70.00   32.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176   57.0000    0.0000 204

  4 omega   32.00   91.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000   90.0000 118

  5 omega  119.00  154.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  125.0000  120.0000 70

  6 omega   32.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000 -120.0000 64

  7 omega   25.00  101.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -94.0000   90.0000 152

  8 omega   36.00  122.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188 -125.0000 -150.0000 172

  9 omega   32.00   83.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000  150.0000 102

 10 omega   27.00   57.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -91.0000  -83.0000 60

 11 omega   90.00  142.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -91.0000  -83.0000 104

 12 omega   39.00   91.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -30.0000   30.0000 104

 13 omega   80.00  153.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   30.0000    0.0000 146

 14 omega   80.00  178.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   30.0000   60.0000 196

 15 omega   37.00  135.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188  -77.0000 -150.0000 196

 16 omega -118.00   -9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -77.0000 -150.0000 218

 17 omega -118.00   -9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -77.0000    0.0000 218

 18 omega -114.00  -13.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -57.0000 -120.0000 202

 19 omega -118.00   -9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6176  -77.0000  120.0000 218

 20 omega   80.00  178.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   30.0000  -90.0000 196

 21 omega   75.00  178.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   77.0000   90.0000 206

 22 omega   55.00  178.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   15.0000 -150.0000 246

 23 omega   35.00  122.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188 -125.0000  -60.0000 174
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0753681000
_diffrn_orient_matrix_UB_12      -0.0096559000
_diffrn_orient_matrix_UB_13      -0.0537169000
_diffrn_orient_matrix_UB_21      -0.0777078000
_diffrn_orient_matrix_UB_22      0.0655589000
_diffrn_orient_matrix_UB_23      0.0271473000
_diffrn_orient_matrix_UB_31      0.0537719000
_diffrn_orient_matrix_UB_32      0.0832375000
_diffrn_orient_matrix_UB_33      -0.0262892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44463
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.3128
_exptl_crystal_size_mid          0.2176
_exptl_crystal_size_min          0.0895
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1301
_refine_ls_number_reflns         15397
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1523P)^2^+10.8256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2578
_refine_ls_wR_factor_ref         0.2670
_reflns_number_gt                12909
_reflns_number_total             15397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401246n_si_002.cif
_cod_data_source_block           2b
_cod_original_cell_volume        4339.00(15)
_cod_database_code               4508353
_reflns_odcompleteness_completeness 99.75
_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
 F21B-P4
 1.55 with sigma of 0.02
 P5B-F26B
 1.58 with sigma of 0.02
 F34A-P6
 1.55 with sigma of 0.02
 F34B-P6
 1.55 with sigma of 0.02
 F36A-P6
 1.55 with sigma of 0.02
 F36B-P6
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O12A \\sim O12B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O13B \\sim O13A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O2B \\sim O2A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O14B \\sim O14A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
F26B \\sim F26A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F25 \\sim P5B \\sim F27: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
C12 \\sim N3 \\sim C10: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
N11 \\sim C45 \\sim C47 \\sim C48 \\sim C49: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13B) \\sim Ueq, Uanis(O13A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14A) \\sim Ueq, Uanis(O14B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F28B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(F36A) \\sim Ueq, Uanis(P6) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32A) \\sim Ueq, Uanis(F32B) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F34A) \\sim Ueq, Uanis(F34B) \\sim Ueq, Uanis(F35A) \\sim Ueq, Uanis(F35B) \\sim Ueq, Uanis(F36B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F21A) = Uanis(F21B)
4. Others
 Sof(O2B)=Sof(H2BA)=Sof(H2BB)=Sof(O5B)=Sof(H5BA)=Sof(H5BB)=Sof(O7B)=Sof(O12B)=
 Sof(H12E)=Sof(H12F)=Sof(O13B)=Sof(H13E)=Sof(H13F)=Sof(O14B)=Sof(H14E)=
 Sof(H14F)=1-FVAR(1)
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=Sof(O5A)=Sof(H5AA)=Sof(H5AB)=Sof(O7A)=Sof(O12A)=
 Sof(H12C)=Sof(H12D)=Sof(O13A)=Sof(H13C)=Sof(H13D)=Sof(O14A)=Sof(H14C)=
 Sof(H14D)=FVAR(1)
 Sof(F32B)=Sof(F34B)=Sof(F35B)=Sof(F36B)=1-FVAR(2)
 Sof(F32A)=Sof(F34A)=Sof(F35A)=Sof(F36A)=FVAR(2)
 Sof(F21B)=1-FVAR(3)
 Sof(F21A)=FVAR(3)
 Sof(P5B)=Sof(F26B)=Sof(F28B)=Sof(F29B)=Sof(F30B)=1-FVAR(4)
 Sof(P5A)=Sof(F26A)=Sof(F28A)=Sof(F29A)=Sof(F30A)=FVAR(4)
 Fixed Uiso: H1C(0.1365) H1D(0.1365) H2AA(0.0765) H2AB(0.0765) H2BA(0.129)
 H2BB(0.129) H3C(0.132) H3D(0.132) H4C(0.1245) H4D(0.1245) H5AA(0.1485)
 H5AB(0.1485) H5BA(0.0735) H5BB(0.0735) H6C(0.33) H6D(0.33) H7AA(0.153)
 H7AB(0.153) H8C(0.273) H8D(0.273) H9C(0.27) H9D(0.27) H10C(0.213) H10D(0.213)
 H11C(0.132) H11D(0.132) H12C(0.0675) H12D(0.0675) H12E(0.1095) H12F(0.1095)
 H13C(0.1425) H13D(0.1425) H13E(0.15) H13F(0.15) H14C(0.147) H14D(0.147)
 H14E(0.111) H14F(0.111)
 Fixed X: H1C(0.57712) H1D(0.63131) H2AA(0.76499) H2AB(0.681561)
 H2BA(0.800509) H2BB(0.79262) H3C(0.92095) H3D(0.942599) H4C(1.07235)
 H4D(1.079989) H5AA(1.27195) H5AB(1.19311) H5BA(1.15689) H5BB(1.22971)
 H6C(1.44735) H6D(1.34662) H7AA(1.400169) H7AB(1.43882) H8C(0.56237)
 H8D(0.5907) H9C(0.54076) H9D(0.641041) H10C(0.26431) H10D(0.24896)
 H11C(0.066689) H11D(0.103291) H12C(-0.073421) H12D(-0.056331) H12E(-0.069011)
 H12F(-0.065081) H13C(-0.21768) H13D(-0.292371) H13E(-0.28638) H13F(-0.19504)
 H14C(0.58574) H14D(0.617311) H14E(0.664281) H14F(0.591321)
 Fixed Y: H1C(0.662331) H1D(0.73308) H2AA(0.83858) H2AB(0.89354)
 H2BA(0.822141) H2BB(0.73926) H3C(0.88227) H3D(0.7928) H4C(0.6737) H4D(0.71333)
 H5AA(0.723981) H5AB(0.658041) H5BA(0.746989) H5BB(0.772969) H6C(0.63254)
 H6D(0.613021) H7AA(0.40212) H7AB(0.4698) H8C(-0.03089) H8D(-0.092931)
 H9C(0.12042) H9D(0.11231) H10C(0.761901) H10D(0.79031) H11C(0.83712)
 H11D(0.79784) H12C(0.634689) H12D(0.727449) H12E(0.62633) H12F(0.711221)
 H13C(0.67917) H13D(0.605981) H13E(0.660911) H13F(0.691821) H14C(-0.15985)
 H14D(-0.245451) H14E(-0.24852) H14F(-0.179699)
 Fixed Z: H1C(1.02203) H1D(0.994449) H2AA(0.982759) H2AB(1.001121)
 H2BA(0.994809) H2BB(1.025861) H3C(0.9312) H3D(0.95272) H4C(0.99234)
 H4D(0.937849) H5AA(0.87429) H5AB(0.88515) H5BA(0.85694) H5BB(0.902789)
 H6C(0.96418) H6D(0.93722) H7AA(0.876469) H7AB(0.917089) H8C(0.5694)
 H8D(0.613941) H9C(0.532169) H9D(0.56149) H10C(0.42317) H10D(0.36567)
 H11C(0.48354) H11D(0.432859) H12C(0.42031) H12D(0.439408) H12E(0.43162)
 H12F(0.46282) H13C(0.49174) H13D(0.49169) H13E(0.52555) H13F(0.4999)
 H14C(0.52349) H14D(0.50009) H14E(0.50851) H14F(0.52272)
5.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), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;