Hexanuclear Cylinder-Shaped Assemblies of Silver and Gold from Benzene‒Hexa-N-heterocyclic Carbenes
Segarra, Candela; Guisado-Barrios, Gregorio; Hahn, F. Ekkehardt; Peris, Eduardo; Organometallics 33 (2014) 5077–; doi:10.1021/om500729b

data_4089671
_publ_section_title
;
 Hexanuclear Cylinder-Shaped Assemblies of Silver and Gold from
 Benzene--Hexa-N-heterocyclic Carbenes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5077
_journal_paper_doi               10.1021/om500729b
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C72 H84 Ag6 N24'
_chemical_formula_sum            'C72 H84 Ag6 B6 F24 N24'
_chemical_formula_weight         2453.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2014-08-26 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.9670(10)
_cell_length_b                   28.073(2)
_cell_length_c                   16.2980(10)
_cell_measurement_temperature    293(2)
_cell_volume                     10508.2(11)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.782
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.782
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19719
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.046
_diffrn_reflns_theta_min         3.392
_exptl_absorpt_coefficient_mu    1.187
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.137
_refine_diff_density_max         1.678
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4992
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          1.703
_refine_ls_shift/su_mean         0.077
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1742P)^2^+40.9068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2760
_refine_ls_wR_factor_ref         0.3086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3296
_reflns_number_total             4992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500729b_si_002.cif
_cod_data_source_block           platon_sq
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               4089671
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed U12: Ag2(0)
 Fixed U23: Ag2(0)
 Fixed Uiso: H14(0.203) H15(0.174) H16A(0.196) H16B(0.196) H17A(0.373)
 H17B(0.373) H17C(0.373) H24(0.212) H25(0.157) H26A(0.281) H26B(0.281)
 H27A(0.833) H27B(0.833) H27C(0.833) H34(0.18) H35(0.144) H36A(0.234)
 H36B(0.234) H37A(0.961) H37B(0.961) H37C(0.961)
 Fixed X: Ag2(0) H14(0.1988) H15(0.21) H16A(0.0532) H16B(0.0983) H17A(0.1145)
 H17B(0.1176) H17C(0.168) H24(0.1833) H25(0.2064) H26A(0.1004) H26B(0.0416)
 H27A(0.011) H27B(0.0724) H27C(0.0595) H34(0.1789) H35(0.2003) H36A(0.0332)
 H36B(0.0773) H37A(0.1475) H37B(0.1318) H37C(0.0926)
 Fixed Y: H14(0.0989) H15(0.1473) H16A(0.1178) H16B(0.0759) H17A(0.1642)
 H17B(0.1135) H17C(0.1311) H24(0.0781) H25(0.1568) H26A(0.0138) H26B(0.0386)
 H27A(0.043) H27B(0.0596) H27C(0.0052) H34(0.2347) H35(0.2626) H36A(0.1787)
 H36B(0.2051) H37A(0.1396) H37B(0.1279) H37C(0.1086)
 Fixed Z: Ag2(0.25) H14(0.0449) H15(0.1671) H16A(-0.047) H16B(-0.0439) H17A(-
 0.1275) H17B(-0.1674) H17C(-0.1101) H24(0.4064) H25(0.3624) H26A(0.3434)
 H26B(0.3184) H27A(0.4521) H27B(0.4829) H27C(0.4708) H34(0.5881) H35(0.4509)
 H36A(0.6018) H36B(0.6613) H37A(0.6553) H37B(0.5639) H37C(0.6353)
;
_shelx_fab_checksum              95773
_olex2_computing_structure_refinement_long 'ShelXL-1997 (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS-1997 (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'