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_4086007
_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         'C128 H128 Ag4 N20, 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C130 H131 Ag4 F24 N21 P4'
_chemical_formula_weight         2998.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.125(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5804(18)
_cell_length_b                   35.051(4)
_cell_length_c                   23.265(2)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.35
_cell_volume                     14155(2)
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            153839
_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         1.309
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1347 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8737.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             6088
_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 20 acetonitrile  molecules 
which have been treated as a diffuse contribution to 
the overall scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         2.379
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1649
_refine_ls_number_reflns         24948
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0926P)^2^+61.8830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19252
_reflns_number_total             24948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00188_si_006.cif
_cod_data_source_block           n140707c
_cod_depositor_comments
'Adding full bibliography for 4086005--4086009.cif.'
_cod_original_cell_volume        14155(3)
_cod_database_code               4086007
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.888
_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
 C129-C130
 1.54 with sigma of 0.01
 N21-C129
 1.22 with sigma of 0.01
3. Rigid bond restraints
 C61, C62
 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 C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C19 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
C112 \\sim C111 \\sim C116 \\sim C115 \\sim C114 \\sim C113: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C130) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F14) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F6) \\sim Ueq, 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(F22) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F20)
\\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F23) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C130) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(C62) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F16) \\sim Ueq,
Uanis(F18) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F22) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C18(H18A,H18B), C25(H25A,H25B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
  C46(H46A,H46B), C53(H53A,H53B), C54(H54A,H54B), C58(H58A,H58B), C71(H71A,
 H71B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B),
 C82(H82A,H82B), C89(H89A,H89B), C104(H10A,H10B), C105(H10C,H10D), C106(H10E,
 H10F), C110(H11C,H11D), C117(H11E,H11F), C118(H11G,H11H), C122(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C15(H15), C16(H16),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30),
  C31(H31), C35(H35), C36(H36), C37(H37), C38(H38), C43(H43), C44(H44),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C72(H72), C73(H73), C79(H79), C80(H80), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88), C92(H92), C93(H93), C94(H94), C95(H95),
 C99(H99), C100(H100), C101(H101), C102(H102), C107(H107), C108(H108),
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C119(H119),
 C120(H120), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128)
5.c Idealised Me refined as rotating group:
 C130(H13C,H13D,H13E)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'