Synthesis and crystal structures of twisted three-dimensional assemblies of adamantane-bridged tris-NHC ligands and AgI
Tominaga, Masahide; Kawaguchi, Taichi; Ohara, Kazuaki; Yamaguchi, Kentaro; Masu, Hyuma; Azumaya, Isao; CrystEngComm 18 (2016) 266–; doi:10.1039/C5CE01860A

data_7223590
_publ_section_title
;
 Synthesis and crystal structures of twisted three-dimensional assemblies
 of adamantane-bridged tris-NHC ligands and AgI
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              266
_journal_paper_doi               10.1039/C5CE01860A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C86 H92 Ag3 N12, 6(C4 H8 O2), 3(F6 P)'
_chemical_formula_sum            'C110 H140 Ag3 F18 N12 O12 P3'
_chemical_formula_weight         2580.85
_chemical_name_common            cageAg3PF6
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-12-02 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.6780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.813(3)
_cell_length_b                   20.6402(19)
_cell_length_c                   16.3040(15)
_cell_measurement_temperature    150
_cell_volume                     11429.6(18)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            55296
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.463
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
The unit cell contains eight molecules of 1,4-dioxane which have 44 electrons 
and have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.630
_refine_diff_density_min         -0.694
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         22635
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0707
_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^)+(0.1242P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                11439
_reflns_number_total             22635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01860a2.cif
_cod_data_source_block           p21c
_cod_database_code               7223590
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              2878