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_7223591
_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_sum            'C16 H16 Ag0.4 F2.4 N1.73 O0.53 P0.4'
_chemical_formula_weight         342.24
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-27 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.187(2)
_cell_angle_gamma                90
_cell_formula_units_Z            30
_cell_length_a                   19.0224(7)
_cell_length_b                   15.7764(7)
_cell_length_c                   38.4287(15)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.0895
_cell_measurement_theta_min      2.9704
_cell_volume                     11272.7(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v4.2.3'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    XP
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'D8 Venture Ultra'
_diffrn_measurement_method       '\f and \w, two \theta position'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_laue_measured_fraction_full 0.989
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            101361
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.265
_diffrn_reflns_theta_max         65.265
_diffrn_reflns_theta_min         3.659
_diffrn_source                   'rotation anode'
_exptl_absorpt_coefficient_mu    5.306
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5244
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.566
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1469
_refine_ls_number_reflns         19114
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0738P)^2^+31.8329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15141
_reflns_number_total             19114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01860a2.cif
_cod_data_source_block           p21c
_cod_original_formula_sum        'C16 H16 Ag0.40 F2.40 N1.73 O0.53 P0.40'
_cod_database_code               7223591
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.328
_shelx_estimated_absorpt_t_max   0.676
_shelx_res_checksum              44948