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_4508351
_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
'4(F3.33 P0.26), 4(C27 H45 N6), F6 P1, 12(H3 O), 12(F1.33 P0.13), 12(F3.67 P0.71), 4(F2.67 P0.74)'
_chemical_formula_sum            'C108 H204 F90 N24 O12 P15'
_chemical_formula_weight         4205.50
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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            8
_cell_length_a                   37.5461(3)
_cell_length_b                   37.5461(3)
_cell_length_c                   37.5461(3)
_cell_measurement_reflns_used    3063
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.3490
_cell_measurement_theta_min      3.3266
_cell_volume                     52929.1(7)
_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
;
SHELXL, 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 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
  1 omega  -31.00   22.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8676   77.0000    0.0000 106

  2 omega   86.00  166.00   0.5000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      107.8188   77.0000  -30.0000 160
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0355647000
_diffrn_orient_matrix_UB_12      0.0038634000
_diffrn_orient_matrix_UB_13      -0.0202261000
_diffrn_orient_matrix_UB_21      0.0058779000
_diffrn_orient_matrix_UB_22      -0.0405143000
_diffrn_orient_matrix_UB_23      0.0025642000
_diffrn_orient_matrix_UB_31      -0.0197026000
_diffrn_orient_matrix_UB_32      -0.0051850000
_diffrn_orient_matrix_UB_33      -0.0355561000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            10627
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.52
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.705
_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    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             17208
_exptl_crystal_size_max          0.2943
_exptl_crystal_size_mid          0.1886
_exptl_crystal_size_min          0.1270
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.751
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.788
_refine_ls_R_factor_all          0.1741
_refine_ls_R_factor_gt           0.1595
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4185
_refine_ls_wR_factor_ref         0.4428
_reflns_number_gt                1619
_reflns_number_total             2517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401246n_si_002.cif
_cod_data_source_block           1b
_cod_database_code               4508351
_chemical_oxdiff_formula         'C27 H30 N6 O6 F18 P3'
_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) groups, All C(H,H) groups
2. Restrained distances
 F4-P2
 1.55 with sigma of 0.02
 F5B-P2
 1.55 with sigma of 0.02
 F5A-P2
 1.55 with sigma of 0.02
 H1C-O1
 0.85 with sigma of 0.02
 N1-H1C
 2.08 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F4 \\sim P2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.08
N1 \\sim N2 \\sim C4 \\sim C3: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(F5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F4) \\sim Ueq, Uanis(P2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F8B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(P1B)=0.16667*(1-FVAR(2))
 Sof(P1A)=0.16667*FVAR(2)
 Fixed Sof: H5A(0.5) H5B(0.5) H3B(0.5) H3A(0.5) H4A(0.5) H4B(0.5) P3B(0.0625)
 F7B(0.5) F10A(0.33333) F8A(0.25) P3A(0.35412) F8B(0.04176) F5B(0.0625)
 F5A(0.02084) F6B(0.125) F7A(0.25) F3A(0.375) F2A(0.125) F1A(0.05556)
 F2B(0.2222) F1B(0.1111) F3B(0.1111)
 Fixed Uiso: H1C(0.3) H1D(0.3)
 Fixed X: H1C(0.16448) H1D(0.194901)
 Fixed Y: H1C(0.46936) H1D(0.48934)
 Fixed Z: H1C(0.2807) H1D(0.28702)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3B,H3A), C2(H2B,H2A), C1(H1B,H1A), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7)
;