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_4086006
_publ_section_title
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 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         'Hg I4, C22 H30 N5'
_chemical_formula_sum            'C22 H30 Hg I4 N5'
_chemical_formula_weight         1072.70
_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                 93.777(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4478(11)
_cell_length_b                   18.521(2)
_cell_length_c                   17.671(2)
_cell_measurement_reflns_used    7059
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.77
_cell_measurement_theta_min      2.48
_cell_volume                     3085.4(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15541
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.595
_exptl_absorpt_coefficient_mu    9.009
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1400 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.3483.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.846
_refine_diff_density_min         -2.790
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5443
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.267
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0710P)^2^+70.3972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4631
_reflns_number_total             5443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00188_si_002.cif
_cod_data_source_block           n130817b
_cod_depositor_comments
'Adding full bibliography for 4086005--4086009.cif.'
_cod_database_code               4086006
_shelx_estimated_absorpt_t_max   0.365
_shelx_estimated_absorpt_t_min   0.310
_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
 Hg1'-I1' = Hg1'-I2' = Hg1'-I3' = Hg1'-I4'
 2.73 with sigma of 0.02
 Hg1-I1 = Hg1-I2 = Hg1-I3 = Hg1-I4
 2.73 with sigma of 0.02
 C14-C15
 1.48 with sigma of 0.01
 N3-C14
 1.5 with sigma of 0.01
 C10-N2
 1.53 with sigma of 0.01
 C9-C10
 1.53 with sigma of 0.01
 N1-C9
 1.38 with sigma of 0.01
 I1'-I2' \\sim I1'-I3' \\sim I1'-I4' \\sim I2'-I3' \\sim I2'-I4' \\sim I3'-I4'
 with sigma of 0.01
 I1-I2 \\sim I1-I3 \\sim I1-I4 \\sim I2-I3 \\sim I2-I4 \\sim I3-I4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C13 \\sim N2 \\sim C11 \\sim C12 \\sim N3: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I2') \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(Hg1) = Uanis(Hg1')
Uanis(I1) = Uanis(I1')
Uanis(I2) = Uanis(I2')
Uanis(I3) = Uanis(I3')
Uanis(I4) = Uanis(I4')
4. Others
 Sof(Hg1')=Sof(I1')=Sof(I2')=Sof(I3')=Sof(I4')=1-FVAR(1)
 Sof(Hg1)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(I4)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B), C16(H16A,H16B),
 C17(H17A,H17B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C18(H18),
 C19(H19), C20(H20)
5.c Fitted pentagon refined as free rotating group:
 N2(C11,C12,N3,C13)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'