Self-assembly of a “Cationic-Cage” via formation of Ag-carbene bonds followed by imine condensation
Mukherjee, Partha Sarathi; Modak, Ritwik; Howlader, Prodip; Mondal, Bijnaneswar; Chemical Communications  (2019) –; doi:10.1039/C9CC02341K

data_7123438
_publ_section_title
;
 Self-assembly of a &#x201C;Cationic-Cage&#x201D; via formation of
 Ag-carbene bonds followed by imine condensation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02341K
_journal_year                    2019
_chemical_formula_moiety         'C78 H59 Ag3 N12 O6, 3(F6 P)'
_chemical_formula_sum            'C78 H59 Ag3 F18 N12 O6 P3'
_chemical_formula_weight         2018.89
_chemical_name_systematic        OC-Ag
_chemical_properties_physical    Air-sensitive,Light-sensitive
_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_date             2018-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-03-05 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.633(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5748(18)
_cell_length_b                   21.1941(18)
_cell_length_c                   19.7887(17)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.87
_cell_volume                     8628.6(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            222247
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.817
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1079 before and 0.0828 after correction.
The Ratio of minimum to maximum transmission is 0.7790.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             4028
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         15165
_refine_ls_number_restraints     1095
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0821P)^2^+67.9323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10041
_reflns_number_total             15165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02341k2.cif
_cod_data_source_block           OC-Ag
_cod_database_code               7123438
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(F03E)=Sof(F03C)=Sof(F0)=Sof(F1)=Sof(F02{)=Sof(F2)=Sof(P0)=1-FVAR(1)
 Sof(P008)=Sof(F02Z)=Sof(F03B)=Sof(F03D)=Sof(F032)=Sof(F034)=Sof(F039)=FVAR(1)
 Sof(O3A)=1-FVAR(2)
 Sof(O3)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C02K(H02E,H02K), C022(H02M,H02R), C023(H02S,H02W), C025(H02X,H02Z), C027(H02,
 H), C029(H0AA,HA)
4.b Aromatic/amide H refined with riding coordinates:
 C00U(H00U), C00W(H00W), C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I),
 C01K(H01K), C01L(H01L), C01N(H01N), C01Q(H01Q), C01T(H01T), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C02A(H02A), C02B(H02B),
 C02C(H02C), C02D(H02D), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02J(H02J), C02L(H02L), C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q),
 C02T(H02T), C02U(H02U), C02V(H02V), C02Y(H02Y), C03C(H03C), C013(H013),
 C017(H017), C019(H019), C020(H020), C021(H021), C024(H024), C026(H026),
 C030(H030), C031(H031), C033(H033), C036(H036), C037(H037)
;
_shelx_res_checksum              1928
_shelx_fab_checksum              88237
_olex2_submission_special_instructions 'No special instructions were received'