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_4086005
_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
'C120 H128 Ag4 N20, 4(F6 P), 3(C2 H3 N), 0.4(C2 O2)'
_chemical_formula_sum            'C129.2 H137 Ag4 F24 N23 O0.8 P4'
_chemical_formula_weight         3036.17
_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             2015-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                76.743(2)
_cell_angle_beta                 78.461(3)
_cell_angle_gamma                69.057(2)
_cell_formula_units_Z            1
_cell_length_a                   14.8817(18)
_cell_length_b                   15.6147(18)
_cell_length_c                   16.1733(19)
_cell_measurement_reflns_used    3268
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.11
_cell_measurement_theta_min      2.36
_cell_volume                     3387.5(7)
_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      296.15
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19720
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.418
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.8324.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6068
_reflns_number_total             11951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00188_si_004.cif
_cod_data_source_block           n131225c
_cod_depositor_comments
'Adding full bibliography for 4086005--4086009.cif.'
_cod_original_formula_sum        'C129.20 H137 Ag4 F24 N23 O0.80 P4'
_cod_database_code               4086005
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H64A,H64B,H64C} of C64, {H62A,H62B,H62C} of C62, {H49A,
  H49B,H49C} of C49, {H60A,H60B,H60C} of C60, All C(H,H) groups
 At 1.5 times of:
  {H1A,H1B,H1C} of C1, {H22A,H22B,H22C} of C22
2. Restrained distances
 N11-C62 = N12-C64
 2.65 with sigma of 0.01
 C62-C61 = C64-C63
 1.47 with sigma of 0.01
 N11-C61 = N12-C63
 1.15 with sigma of 0.01
 O1-C65
 1.48 with sigma of 0.01
 H38A-H29
 2 with sigma of 0.01
3. Rigid bond restraints
 P1, F5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, F7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C59, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(N12)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F7) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim
Ueq, Uanis(F12) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(P2) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F6) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Fixed Sof: N12(0.5) C63(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) O1(0.4)
 C65(0.4)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C21(H21A,H21B), C23(H23A,H23B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C59(H59A,H59B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C17(H17), C18(H18), C19(H19), C20(H20),
 C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35), C36(H36),
  C44(H44), C45(H45), C46(H46), C47(H47), C55(H55), C56(H56), C57(H57), C58(H58)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C49(H49A,H49B,H49C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'