First homoleptic MIC and heteroleptic NHC-MIC coordination cages from 1,3,5-triphenylbenzene-bridged tris-MIC and tris-NHC ligands.
Mejuto, Carmen; Guisado-Barrios, Gregorio; Gusev, Dmitry; Peris, Eduardo; Chemical communications (Cambridge, England) 51 (2015) 13914–13917; doi:10.1039/c5cc05114b

data_7117766
_publ_section_title
;
 First homoleptic MIC and heteroleptic NHC-MIC coordination cages from
 1,3,5-triphenylbenzene-bridged tris-MIC and tris-NHC ligands.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13914
_journal_page_last               13917
_journal_paper_doi               10.1039/c5cc05114b
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C168 H162 Ag3 N18, 3(F6 P)'
_chemical_formula_sum            'C168 H162 Ag3 F18 N18 P3'
_chemical_formula_weight         3191.67
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
'Air-sensitive, Heat-sensitive, Light-sensitive'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-14 deposited with the CCDC.
2015-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   35.4661(16)
_cell_length_b                   35.4661(16)
_cell_length_c                   26.1940(17)
_cell_measurement_reflns_used    3987
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      64.9440
_cell_measurement_theta_min      4.1040
_cell_volume                     28534(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega  -74.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   77.0000  -90.0000 120

  2 omega    2.00  122.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       37.6057   77.0000  150.0000 120

  3 omega  100.00  178.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8683   77.0000 -120.0000 78

  4 omega   95.00  178.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8683   77.0000  -90.0000 83

  5 omega   66.00  178.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8683   77.0000 -180.0000 112

  6 omega   95.00  178.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8683   77.0000  -60.0000 83

  7 omega  -49.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   37.0000  120.0000 91

  8 omega -117.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -37.0000  -30.0000 111

  9 omega  100.00  125.00   1.0000  275.0000
omega____ theta____ kappa____ phi______ frames
    -      101.8683  111.0000   90.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0332451000
_diffrn_orient_matrix_UB_12      0.0158859000
_diffrn_orient_matrix_UB_13      0.0440671000
_diffrn_orient_matrix_UB_21      -0.0230887000
_diffrn_orient_matrix_UB_22      -0.0461715000
_diffrn_orient_matrix_UB_23      0.0230116000
_diffrn_orient_matrix_UB_31      0.0296530000
_diffrn_orient_matrix_UB_32      -0.0114144000
_diffrn_orient_matrix_UB_33      -0.0315606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_laue_measured_fraction_full 0.918
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36807
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         64.937
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_F_000             9864
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.1117
_exptl_crystal_size_mid          0.1056
_exptl_crystal_size_min          0.0466
_platon_squeeze_details
;
;
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10546
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1644P)^2^+33.6004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2561
_refine_ls_wR_factor_ref         0.2886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6439
_reflns_number_total             10546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc05114b2.cif
_cod_data_source_block           str1725
_cod_database_code               7117766
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C168 H144 N18 Ag3 P F6'
_reflns_odcompleteness_completeness 97.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F4 \\sim P1-F6
 with sigma of 0.02
 P1-F5 \\sim P1-F3 \\sim P1-F2 \\sim P1-F1
 with sigma of 0.02
 F3-F2 \\sim F4-F1 \\sim F6-F5
 with sigma of 0.02
 P1-F2 \\sim P1-F1 \\sim P1-F3 \\sim P1-F5 \\sim P1-F6A \\sim P1-F4 \\sim P1-F6
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F3 \\sim F5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F1 \\sim F2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Others
 Fixed Sof: F6(0.5) F6A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C7'(H7'), C8(H8), C8'(H8'), C10(H10), C10'(H10'), C11(H11),
 C11'(H11'), C13(H13), C13'(H13'), C16(H16), C16'(H16'), C18(H18), C18'(H18'),
 C25(H25), C25'(H25'), C27(H27), C27'(H27')
6.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F), C21(H21A,H21B,H21C), C21'(H21D,
 H21E,H21F), C22(H22A,H22B,H22C), C22'(H22D,H22E,H22F), C29(H29A,H29B,H29C),
 C29'(H29D,H29E,H29F), C30(H30A,H30B,H30C), C30'(H30D,H30E,H30F), C31(H31A,H31B,
 H31C), C31'(H31D,H31E,H31F)
;
_olex2_submission_special_instructions 'No special instructions were received'