NHC Tetranuclear Silver(I) Complexes and Intramolecular Extended π‒π Interactions
Liu, Qing-Xiang; Huo, Ran; Liu, Jun; Wei, Qing; Zhao, Xiao-Jun; Zhao, Zhi-Xiang; Organometallics 34 (2015) 3167–; doi:10.1021/acs.organomet.5b00188

data_4086009
_publ_section_title
;
 NHC Tetranuclear Silver(I) Complexes and Intramolecular Extended \p--\p
 Interactions
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3167
_journal_paper_doi               10.1021/acs.organomet.5b00188
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C80 H80 Ag4 N14 O2 S2, C2 H4 Cl2, 4(F6 P)'
_chemical_formula_sum            'C82 H84 Ag4 Cl2 F24 N14 O2 P4 S2'
_chemical_formula_weight         2444.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.6740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1029(10)
_cell_length_b                   24.1284(11)
_cell_length_c                   22.9785(11)
_cell_measurement_reflns_used    9369
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.24
_cell_volume                     10873.0(9)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '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  0.0360
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31201
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.338
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0843 before and 0.0437 after correction.
The Ratio of minimum to maximum transmission is 0.8876.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The unit cell contains 8 dichloroethane and 4 DMSO molecules 
which have been treated as a diffuse contribution to 
the overall scattering without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         9578
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0708P)^2^+5.3705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7229
_reflns_number_total             9578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00188_si_003.cif
_cod_data_source_block           n130901b
_cod_depositor_comments
'Adding full bibliography for 4086005--4086009.cif.'
_cod_database_code               4086009
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.848
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C40-C39 = C40'-C39'
 2.7 with sigma of 0.01
 S1-C39 = S1-C40 = S1'-C39' = S1'-C40'
 1.75 with sigma of 0.01
 O1-S1 = O1'-S1'
 1.46 with sigma of 0.01
 O1'-C39' \\sim O1'-C40'
 with sigma of 0.001
 O1-C39 \\sim O1-C40
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40')
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C39) = Uanis(C39')
Uanis(C40) = Uanis(C40')
4. Others
 Sof(O1')=Sof(S1')=Sof(C39')=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40')=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(O1)=Sof(S1)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C25(H25A,H25B), C31(H31A,H31B), C41(H41A,H41B)
5.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11),
 C12(H12), C20(H20), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29),
  C30(H30), C35(H35), C36(H36), C37(H37)
5.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C39'(H39D,H39E,H39F), C40'(H40D,
 H40E,H40F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'