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_4086008
_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         'C52 H72 Ag2 N10, 2(F6 P)'
_chemical_formula_sum            'C52 H72 Ag2 F12 N10 P2'
_chemical_formula_weight         1342.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                105.738(3)
_cell_angle_beta                 96.198(3)
_cell_angle_gamma                102.474(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6665(17)
_cell_length_b                   15.880(2)
_cell_length_c                   20.137(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3450.5(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19313
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.067
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.8263.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.262
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         12113
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2287
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7462
_reflns_number_total             12113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00188_si_005.cif
_cod_data_source_block           n140604c_sqd
_cod_depositor_comments
'Adding full bibliography for 4086005--4086009.cif.'
_cod_original_cell_volume        3450.6(9)
_cod_database_code               4086008
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.887
_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
 C15-C17 = C16-C18 = C49-C51 = C50-C52
 2.54 with sigma of 0.01
 C4-C2 = C4'-C2' = C3-C1 = C3'-C1'
 2.54 with sigma of 0.01
 N1-C3 = N1-C3' = N5-C16 = N10-C50
 2.5 with sigma of 0.01
 C15-C16 = C16-C17 = C17-C18 = C49-C50 = C50-C51 = C51-C52
 1.53 with sigma of 0.01
 C4-C3 = C4'-C3' = C3-C2 = C3'-C2' = C2-C1 = C2'-C1'
 1.53 with sigma of 0.01
 N1-C4 = N1-C4' = N5-C15 = N10-C49
 1.46 with sigma of 0.005
 C15-C17 = C15'-C17' = C16-C18 = C16'-C18'
 2.54 with sigma of 0.01
 N5-C16 = N5-C16'
 2.46 with sigma of 0.01
 C17-C18 = C17'-C18'
 1.53 with sigma of 0.01
 C15-C16 = C16-C17 = C15'-C16' = C16'-C17'
 1.51 with sigma of 0.01
 N5-C15 = N5-C15'
 1.47 with sigma of 0.01
3. Rigid bond restraints
 C16', C15'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16', C17'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N10, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ag2, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C48, Ag2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C1' \\sim C2' \\sim C3' \\sim C4': within 1.7A with sigma of 0.005 and sigma
for terminal atoms of 0.01
N10 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C18) \\sim Ueq, Uanis(C18') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C4) \\sim Ueq, Uanis(C4') \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C16) \\sim Ueq, Uanis(C16') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17) \\sim Ueq, Uanis(C17') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C4) = Uanis(C4')
Uanis(C3) = Uanis(C3')
Uanis(C2) = Uanis(C2')
Uanis(C1) = Uanis(C1')
Uanis(C18) = Uanis(C18')
Uanis(C17) = Uanis(C17')
Uanis(C16) = Uanis(C16')
Uanis(C15) = Uanis(C15')
5. Others
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(H1'C)=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(C3')=
 Sof(H3'A)=Sof(H3'B)=Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(C15')=Sof(H15C)=Sof(H15D)=
 Sof(C16')=Sof(H16C)=Sof(H16D)=Sof(C17')=Sof(H17C)=Sof(H17D)=Sof(C18')=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C2'(H2'A,H2'B), C3'(H3'A,H3'B),
 C4'(H4'A,H4'B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C15'(H15C,H15D), C16'(H16C,
 H16D), C17'(H17C,H17D), C19(H19A,H19B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B),
  C45(H45A,H45B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
6.b Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C12(H12), C13(H13), C22(H22), C23(H23), C24(H24), C25(H25),
 C29(H29), C30(H30), C31(H31), C32(H32), C37(H37), C38(H38), C46(H46), C47(H47)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1'(H1'A,H1'B,H1'C), C18(H18A,H18B,H18C), C18'(H18D,H18E,
 H18F), C43(H43A,H43B,H43C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20