#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/23/7222352.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7222352
loop_
_publ_author_name
'Alen, Jo'
'Van Meervelt, Luc'
'Dehaen, Wim'
'Dobrzańska, Liliana'
_publ_section_title
;
 Solvent diffusion through a non-porous crystal ‘caught in the
 act’ and related single-crystal-to-single-crystal transformations
 in a cationic dinuclear Ag(i) complex
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8957
_journal_paper_doi               10.1039/C5CE01348H
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C34 H40 Ag2 N8, 2(F6 Sb)'
_chemical_formula_sum            'C34 H40 Ag2 F12 N8 Sb2'
_chemical_formula_weight         1247.98
_chemical_name_common            work
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-08 deposited with the CCDC.
2015-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                92.845(2)
_cell_angle_beta                 103.284(2)
_cell_angle_gamma                101.842(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9070(4)
_cell_length_b                   9.6544(4)
_cell_length_c                   12.2203(5)
_cell_measurement_temperature    100(2)
_cell_volume                     995.78(7)
_computing_cell_refinement       'SAINT PLUS(Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT PLUS'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'crossed G\"obel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9080
_diffrn_reflns_theta_full        67.75
_diffrn_reflns_theta_max         69.87
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    19.266
_exptl_absorpt_correction_T_max  0.1885
_exptl_absorpt_correction_T_min  0.0566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS in SAINT-Plus (Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+1.1974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                3040
_reflns_number_total             3531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01348h2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7222347--7222352.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7222352
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ag1 Ag 0.71356(5) 1.05068(4) 0.83294(4) 0.03441(13) Uani 1 1 d .
N1 N 0.8870(5) 0.9480(5) 0.8008(4) 0.0314(10) Uani 1 1 d .
C2 C 0.8691(6) 0.8500(6) 0.7167(5) 0.0328(12) Uani 1 1 d .
H2 H 0.7702 0.8058 0.6669 0.039 Uiso 1 1 calc R
N3 N 1.0080(5) 0.8204(5) 0.7103(4) 0.0278(9) Uani 1 1 d .
C4 C 1.1225(6) 0.9034(6) 0.7972(5) 0.0316(12) Uani 1 1 d .
H4 H 1.2326 0.9057 0.8152 0.038 Uiso 1 1 calc R
C5 C 1.0463(7) 0.9816(6) 0.8522(5) 0.0349(12) Uani 1 1 d .
H5 H 1.0955 1.0489 0.9163 0.042 Uiso 1 1 calc R
C6 C 1.0355(6) 0.7090(6) 0.6349(5) 0.0321(12) Uani 1 1 d .
H6A H 1.0633 0.6316 0.6802 0.038 Uiso 1 1 calc R
H6B H 1.1276 0.7500 0.6052 0.038 Uiso 1 1 calc R
C7 C 0.8967(6) 0.6456(6) 0.5361(5) 0.0303(11) Uani 1 1 d .
C8 C 0.8861(6) 0.6953(6) 0.4291(5) 0.0315(12) Uani 1 1 d .
C9 C 0.7720(6) 0.6189(6) 0.3361(5) 0.0317(12) Uani 1 1 d .
C10 C 0.6634(6) 0.4988(6) 0.3490(5) 0.0327(12) Uani 1 1 d .
C11 C 0.6683(6) 0.4586(6) 0.4574(5) 0.0327(12) Uani 1 1 d .
H11 H 0.5893 0.3812 0.4677 0.039 Uiso 1 1 calc R
C12 C 0.7838(7) 0.5273(6) 0.5499(5) 0.0328(12) Uani 1 1 d .
C13 C 0.9972(7) 0.8308(6) 0.4147(6) 0.0399(13) Uani 1 1 d .
H13A H 1.0567 0.8789 0.4892 0.060 Uiso 1 1 calc R
H13B H 0.9358 0.8936 0.3735 0.060 Uiso 1 1 calc R
H13C H 1.0711 0.8075 0.3721 0.060 Uiso 1 1 calc R
C14 C 0.5443(7) 0.4100(7) 0.2485(5) 0.0427(14) Uani 1 1 d .
H14A H 0.4773 0.4693 0.2080 0.064 Uiso 1 1 calc R
H14B H 0.4782 0.3309 0.2748 0.064 Uiso 1 1 calc R
H14C H 0.6002 0.3725 0.1976 0.064 Uiso 1 1 calc R
C15 C 0.7897(10) 0.4777(7) 0.6641(5) 0.0503(18) Uani 1 1 d .
H15A H 0.8766 0.4286 0.6847 0.075 Uiso 1 1 calc R
H15B H 0.6894 0.4122 0.6631 0.075 Uiso 1 1 calc R
H15C H 0.8070 0.5597 0.7197 0.075 Uiso 1 1 calc R
C16 C 0.7771(7) 0.6586(7) 0.2181(5) 0.0354(13) Uani 1 1 d .
H16A H 0.8794 0.7251 0.2224 0.042 Uiso 1 1 calc R
H16B H 0.7730 0.5717 0.1700 0.042 Uiso 1 1 calc R
N17 N 0.6483(5) 0.7248(5) 0.1635(4) 0.0313(10) Uani 1 1 d .
C18 C 0.5640(6) 0.7962(6) 0.2128(5) 0.0325(12) Uani 1 1 d .
H18 H 0.5744 0.8077 0.2921 0.039 Uiso 1 1 calc R
N19 N 0.4643(6) 0.8488(5) 0.1379(4) 0.0364(11) Uani 1 1 d .
C20 C 0.4867(8) 0.8094(8) 0.0346(5) 0.0468(16) Uani 1 1 d .
H20 H 0.4313 0.8313 -0.0363 0.056 Uiso 1 1 calc R
C21 C 0.6013(8) 0.7339(7) 0.0507(5) 0.0455(16) Uani 1 1 d .
H21 H 0.6413 0.6946 -0.0064 0.055 Uiso 1 1 calc R
Sb22 Sb 0.5000 1.0000 0.5000 0.02968(14) Uani 1 2 d S
F23 F 0.4514(7) 0.8948(4) 0.6160(3) 0.0759(15) Uani 1 1 d .
F24 F 0.6565(5) 0.9035(6) 0.4909(4) 0.0777(15) Uani 1 1 d .
F25 F 0.3575(4) 0.8622(4) 0.3904(3) 0.0465(9) Uani 1 1 d .
Sb26 Sb 1.0000 1.5000 1.0000 0.02919(14) Uani 1 2 d S
F27 F 0.9088(4) 1.4058(4) 1.1076(3) 0.0401(8) Uani 1 1 d .
F28 F 1.1914(4) 1.4487(4) 1.0611(3) 0.0445(8) Uani 1 1 d .
F29 F 0.9356(4) 1.3304(4) 0.9029(3) 0.0436(8) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ag1 N19 178.75(19) . 2_676
C2 N1 C5 105.6(5) . .
C2 N1 Ag1 126.4(4) . .
C5 N1 Ag1 127.4(4) . .
N1 C2 N3 111.7(5) . .
N1 C2 H2 124.2 . .
N3 C2 H2 124.2 . .
C2 N3 C4 107.0(5) . .
C2 N3 C6 127.9(5) . .
C4 N3 C6 124.7(4) . .
C5 C4 N3 106.2(5) . .
C5 C4 H4 126.9 . .
N3 C4 H4 126.9 . .
C4 C5 N1 109.5(5) . .
C4 C5 H5 125.2 . .
N1 C5 H5 125.2 . .
N3 C6 C7 114.9(4) . .
N3 C6 H6A 108.5 . .
C7 C6 H6A 108.5 . .
N3 C6 H6B 108.5 . .
C7 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C12 C7 C8 119.6(5) . .
C12 C7 C6 118.9(5) . .
C8 C7 C6 121.3(5) . .
C9 C8 C7 119.4(5) . .
C9 C8 C13 120.2(5) . .
C7 C8 C13 120.4(5) . .
C10 C9 C8 120.9(5) . .
C10 C9 C16 119.4(5) . .
C8 C9 C16 119.4(5) . .
C9 C10 C11 118.4(5) . .
C9 C10 C14 121.7(5) . .
C11 C10 C14 119.8(5) . .
C12 C11 C10 122.0(5) . .
C12 C11 H11 119.0 . .
C10 C11 H11 119.0 . .
C11 C12 C7 119.3(5) . .
C11 C12 C15 120.7(5) . .
C7 C12 C15 120.0(6) . .
C8 C13 H13A 109.5 . .
C8 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C8 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C10 C14 H14A 109.5 . .
C10 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C10 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C12 C15 H15A 109.5 . .
C12 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C12 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N17 C16 C9 114.4(4) . .
N17 C16 H16A 108.7 . .
C9 C16 H16A 108.7 . .
N17 C16 H16B 108.7 . .
C9 C16 H16B 108.7 . .
H16A C16 H16B 107.6 . .
C18 N17 C21 106.6(5) . .
C18 N17 C16 128.1(5) . .
C21 N17 C16 125.2(5) . .
N19 C18 N17 111.7(5) . .
N19 C18 H18 124.2 . .
N17 C18 H18 124.2 . .
C18 N19 C20 105.9(5) . .
C18 N19 Ag1 127.4(4) . 2_676
C20 N19 Ag1 126.3(4) . 2_676
C21 C20 N19 108.4(5) . .
C21 C20 H20 125.8 . .
N19 C20 H20 125.8 . .
C20 C21 N17 107.4(5) . .
C20 C21 H21 126.3 . .
N17 C21 H21 126.3 . .
F24 Sb22 F24 180.000(2) 2_676 .
F24 Sb22 F23 90.2(3) 2_676 2_676
F24 Sb22 F23 89.8(3) . 2_676
F24 Sb22 F23 89.8(3) 2_676 .
F24 Sb22 F23 90.2(3) . .
F23 Sb22 F23 180.0(2) 2_676 .
F24 Sb22 F25 91.41(18) 2_676 .
F24 Sb22 F25 88.59(18) . .
F23 Sb22 F25 88.76(18) 2_676 .
F23 Sb22 F25 91.24(18) . .
F24 Sb22 F25 88.59(18) 2_676 2_676
F24 Sb22 F25 91.41(18) . 2_676
F23 Sb22 F25 91.24(18) 2_676 2_676
F23 Sb22 F25 88.76(18) . 2_676
F25 Sb22 F25 180.000(1) . 2_676
F28 Sb26 F28 180.000(2) 2_787 .
F28 Sb26 F27 89.58(15) 2_787 .
F28 Sb26 F27 90.42(15) . .
F28 Sb26 F27 90.42(15) 2_787 2_787
F28 Sb26 F27 89.58(15) . 2_787
F27 Sb26 F27 180.000(1) . 2_787
F28 Sb26 F29 89.09(16) 2_787 2_787
F28 Sb26 F29 90.91(16) . 2_787
F27 Sb26 F29 90.35(15) . 2_787
F27 Sb26 F29 89.65(15) 2_787 2_787
F28 Sb26 F29 90.91(16) 2_787 .
F28 Sb26 F29 89.09(16) . .
F27 Sb26 F29 89.65(15) . .
F27 Sb26 F29 90.35(15) 2_787 .
F29 Sb26 F29 180.00(14) 2_787 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.096(5) .
Ag1 N19 2.106(5) 2_676
N1 C2 1.320(7) .
N1 C5 1.376(7) .
C2 N3 1.344(7) .
C2 H2 0.9500 .
N3 C4 1.376(7) .
N3 C6 1.475(7) .
C4 C5 1.361(8) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.514(8) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C12 1.404(8) .
C7 C8 1.404(8) .
C8 C9 1.395(8) .
C8 C13 1.514(8) .
C9 C10 1.390(8) .
C9 C16 1.519(7) .
C10 C11 1.393(8) .
C10 C14 1.514(8) .
C11 C12 1.374(8) .
C11 H11 0.9500 .
C12 C15 1.491(8) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 N17 1.470(7) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
N17 C18 1.334(7) .
N17 C21 1.359(8) .
C18 N19 1.320(7) .
C18 H18 0.9500 .
N19 C20 1.369(8) .
N19 Ag1 2.106(5) 2_676
C20 C21 1.356(8) .
C20 H20 0.9500 .
C21 H21 0.9500 .
Sb22 F24 1.848(4) 2_676
Sb22 F24 1.848(4) .
Sb22 F23 1.863(4) 2_676
Sb22 F23 1.863(4) .
Sb22 F25 1.877(3) .
Sb22 F25 1.877(3) 2_676
Sb26 F28 1.873(3) 2_787
Sb26 F28 1.873(3) .
Sb26 F27 1.877(3) .
Sb26 F27 1.877(3) 2_787
Sb26 F29 1.878(3) 2_787
Sb26 F29 1.878(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Ag1 N1 C2 N3 171.0(3) . .
N1 C2 N3 C4 1.0(6) . .
N1 C2 N3 C6 174.1(5) . .
C2 N3 C4 C5 -0.6(6) . .
C6 N3 C4 C5 -174.0(5) . .
N3 C4 C5 N1 0.1(6) . .
C2 N1 C5 C4 0.5(6) . .
Ag1 N1 C5 C4 -171.3(4) . .
C2 N3 C6 C7 15.8(8) . .
C4 N3 C6 C7 -172.2(5) . .
N3 C6 C7 C12 -89.1(6) . .
N3 C6 C7 C8 96.1(6) . .
C12 C7 C8 C9 -5.7(8) . .
C6 C7 C8 C9 169.0(5) . .
C12 C7 C8 C13 174.2(5) . .
C6 C7 C8 C13 -11.1(8) . .
C7 C8 C9 C10 3.5(8) . .
C13 C8 C9 C10 -176.4(5) . .
C7 C8 C9 C16 -170.2(5) . .
C13 C8 C9 C16 9.9(7) . .
C8 C9 C10 C11 1.8(8) . .
C16 C9 C10 C11 175.5(5) . .
C8 C9 C10 C14 -176.7(5) . .
C16 C9 C10 C14 -3.0(8) . .
C9 C10 C11 C12 -5.0(8) . .
C14 C10 C11 C12 173.6(5) . .
C10 C11 C12 C7 2.8(8) . .
C10 C11 C12 C15 -177.3(5) . .
C8 C7 C12 C11 2.6(8) . .
C6 C7 C12 C11 -172.2(5) . .
C8 C7 C12 C15 -177.2(5) . .
C6 C7 C12 C15 7.9(8) . .
C10 C9 C16 N17 76.4(7) . .
C8 C9 C16 N17 -109.8(6) . .
C9 C16 N17 C18 24.7(8) . .
C9 C16 N17 C21 -161.0(6) . .
C21 N17 C18 N19 0.8(7) . .
C16 N17 C18 N19 176.0(5) . .
N17 C18 N19 C20 -0.3(7) . .
N17 C18 N19 Ag1 172.4(4) . 2_676
C18 N19 C20 C21 -0.4(8) . .
Ag1 N19 C20 C21 -173.2(5) 2_676 .
N19 C20 C21 N17 0.8(8) . .
C18 N17 C21 C20 -1.0(8) . .
C16 N17 C21 C20 -176.3(6) . .
