#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/23/7222348.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_7222348
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(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H46 Ag2 B2 F8 N10'
_chemical_formula_weight         1032.21
_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                96.972(7)
_cell_angle_beta                 100.487(6)
_cell_angle_gamma                104.709(7)
_cell_formula_units_Z            1
_cell_length_a                   8.7304(7)
_cell_length_b                   9.6666(9)
_cell_length_c                   13.3193(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1052.33(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15189
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  0.8473
_exptl_absorpt_correction_T_min  0.8013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,Version 1.171.35.21 
(release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46).
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5062
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0790P)²+2.4167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1574
_reflns_number_gt                4095
_reflns_number_total             5062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce01348h2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7222347--7222352.cif.'
_cod_original_cell_volume        1052.33(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7222348
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.00430(4) 0.04452(4) 0.27164(3) 0.03362(15) Uani 1 1 d . . .
N1 N -0.1902(5) 0.1380(5) 0.2569(3) 0.0320(9) Uani 1 1 d . . .
C2 C -0.2385(6) 0.2082(5) 0.1843(4) 0.0315(10) Uani 1 1 d . . .
H2 H -0.1874 0.2274 0.1282 0.038 Uiso 1 1 calc R . .
N3 N -0.3692(5) 0.2489(5) 0.1997(3) 0.0353(9) Uani 1 1 d . . .
C4 C -0.4078(7) 0.2012(7) 0.2873(4) 0.0420(13) Uani 1 1 d . . .
H4 H -0.4951 0.2135 0.3175 0.050 Uiso 1 1 calc R . .
C5 C -0.2960(7) 0.1330(7) 0.3220(4) 0.0430(13) Uani 1 1 d . . .
H5 H -0.2916 0.0886 0.3819 0.052 Uiso 1 1 calc R . .
C6 C -0.4573(6) 0.3320(6) 0.1379(5) 0.0409(12) Uani 1 1 d . . .
H6A H -0.4615 0.4187 0.1841 0.049 Uiso 1 1 calc R . .
H6B H -0.5703 0.2713 0.1087 0.049 Uiso 1 1 calc R . .
C7 C -0.3800(6) 0.3808(6) 0.0496(4) 0.0357(11) Uani 1 1 d . . .
C8 C -0.4376(6) 0.2988(6) -0.0504(4) 0.0375(12) Uani 1 1 d . . .
C9 C -0.3788(6) 0.3532(6) -0.1331(4) 0.0375(11) Uani 1 1 d . . .
C10 C -0.2555(6) 0.4840(6) -0.1145(4) 0.0391(12) Uani 1 1 d . . .
C11 C -0.1923(6) 0.5599(6) -0.0130(4) 0.0363(11) Uani 1 1 d . . .
H11 H -0.1050 0.6464 0.0004 0.044 Uiso 1 1 calc R . .
C12 C -0.2560(6) 0.5103(6) 0.0691(4) 0.0361(11) Uani 1 1 d . . .
C13 C -0.5618(7) 0.1527(6) -0.0700(5) 0.0475(14) Uani 1 1 d . . .
H13A H -0.5512 0.1093 -0.0073 0.071 Uiso 1 1 calc R . .
H13B H -0.5439 0.0891 -0.1272 0.071 Uiso 1 1 calc R . .
H13C H -0.6710 0.1647 -0.0884 0.071 Uiso 1 1 calc R . .
C14 C -0.1898(7) 0.5468(8) -0.2015(5) 0.0489(14) Uani 1 1 d . . .
H14A H -0.1393 0.4801 -0.2354 0.073 Uiso 1 1 calc R . .
H14B H -0.1086 0.6407 -0.1734 0.073 Uiso 1 1 calc R . .
H14C H -0.2788 0.5604 -0.2522 0.073 Uiso 1 1 calc R . .
C15 C -0.1869(7) 0.5979(6) 0.1773(5) 0.0424(12) Uani 1 1 d . . .
H15A H -0.2703 0.6359 0.2014 0.064 Uiso 1 1 calc R . .
H15B H -0.0935 0.6790 0.1763 0.064 Uiso 1 1 calc R . .
H15C H -0.1521 0.5356 0.2242 0.064 Uiso 1 1 calc R . .
C16 C -0.4547(7) 0.2747(7) -0.2441(4) 0.0453(14) Uani 1 1 d . . .
H16A H -0.5636 0.2098 -0.2463 0.054 Uiso 1 1 calc R . .
H16B H -0.4693 0.3473 -0.2886 0.054 Uiso 1 1 calc R . .
N17 N -0.3582(5) 0.1883(5) -0.2868(3) 0.0371(10) Uani 1 1 d . . .
C18 C -0.2524(6) 0.1267(6) -0.2356(4) 0.0339(10) Uani 1 1 d . . .
H18 H -0.2213 0.1390 -0.1622 0.041 Uiso 1 1 calc R . .
N19 N -0.1980(5) 0.0483(5) -0.2997(3) 0.0372(10) Uani 1 1 d . . .
C20 C -0.2740(10) 0.0571(12) -0.3967(5) 0.082(3) Uani 1 1 d . . .
H20 H -0.2596 0.0098 -0.4597 0.098 Uiso 1 1 calc R . .
C21 C -0.3737(9) 0.1439(10) -0.3897(5) 0.068(2) Uani 1 1 d . . .
H21 H -0.4405 0.1685 -0.4454 0.082 Uiso 1 1 calc R . .
B22 B 0.030(2) 0.020(3) 0.0122(17) 0.042(5) Uani 0.50 1 d PDU A -1
F23 F 0.0901(9) -0.0974(7) -0.0126(6) 0.0541(17) Uani 0.50 1 d PU A -1
F24 F 0.0309(8) 0.0923(7) -0.0764(5) 0.0434(15) Uani 0.50 1 d P A -1
F25 F -0.1076(13) -0.0236(14) 0.0373(9) 0.090(3) Uani 0.50 1 d PDU A -1
F26 F 0.1439(11) 0.1113(8) 0.0927(5) 0.060(2) Uani 0.50 1 d PD A -1
B27 B -0.470(2) 0.463(3) 0.4877(13) 0.114(7) Uani 0.50 1 d PDU B -1
F28 F -0.3338(12) 0.4491(12) 0.5390(7) 0.080(3) Uani 0.50 1 d PD B -1
F29 F -0.4327(11) 0.5125(9) 0.3962(7) 0.072(2) Uani 0.50 1 d PU B -1
F30 F -0.509(3) 0.564(3) 0.5424(17) 0.152(5) Uani 0.50 1 d PU B -1
F31 F -0.5892(12) 0.3395(10) 0.4552(8) 0.072(2) Uani 0.50 1 d PD B -1
N32 N -0.1592(7) -0.1380(6) 0.4098(4) 0.0519(13) Uani 1 1 d . . .
C33 C -0.1179(8) -0.2301(8) 0.4380(5) 0.0537(15) Uani 1 1 d . . .
C34 C -0.0624(15) -0.3485(9) 0.4738(7) 0.092(3) Uani 1 1 d . . .
H34A H 0.0275 -0.3606 0.4423 0.138 Uiso 1 1 calc R . .
H34B H -0.1519 -0.4384 0.4539 0.138 Uiso 1 1 calc R . .
H34C H -0.0251 -0.3264 0.5495 0.138 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
N19 Ag1 N1 175.17(15) 2 .
C2 N1 C5 106.1(4) . .
C2 N1 Ag1 128.3(3) . .
C5 N1 Ag1 125.6(3) . .
N1 C2 N3 111.1(5) . .
N1 C2 H2 124.5 . .
N3 C2 H2 124.5 . .
C2 N3 C4 107.5(4) . .
C2 N3 C6 128.1(5) . .
C4 N3 C6 124.4(4) . .
C5 C4 N3 106.0(4) . .
C5 C4 H4 127.0 . .
N3 C4 H4 127.0 . .
C4 C5 N1 109.3(5) . .
C4 C5 H5 125.3 . .
N1 C5 H5 125.3 . .
N3 C6 C7 113.1(4) . .
N3 C6 H6A 109.0 . .
C7 C6 H6A 109.0 . .
N3 C6 H6B 109.0 . .
C7 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
C12 C7 C8 120.6(5) . .
C12 C7 C6 119.2(5) . .
C8 C7 C6 120.1(5) . .
C7 C8 C9 119.6(5) . .
C7 C8 C13 120.6(5) . .
C9 C8 C13 119.8(5) . .
C10 C9 C8 120.1(5) . .
C10 C9 C16 119.6(5) . .
C8 C9 C16 120.3(5) . .
C11 C10 C9 119.4(5) . .
C11 C10 C14 118.9(5) . .
C9 C10 C14 121.7(5) . .
C12 C11 C10 120.8(5) . .
C12 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
C7 C12 C11 119.3(5) . .
C7 C12 C15 121.7(5) . .
C11 C12 C15 119.0(5) . .
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 113.6(4) . .
N17 C16 H16A 108.8 . .
C9 C16 H16A 108.8 . .
N17 C16 H16B 108.8 . .
C9 C16 H16B 108.8 . .
H16A C16 H16B 107.7 . .
C18 N17 C21 107.2(4) . .
C18 N17 C16 128.5(5) . .
C21 N17 C16 124.0(4) . .
N19 C18 N17 111.4(4) . .
N19 C18 H18 124.3 . .
N17 C18 H18 124.3 . .
C18 N19 C20 105.8(4) . .
C18 N19 Ag1 130.1(4) . 2
C20 N19 Ag1 123.2(4) . 2
C21 C20 N19 109.7(6) . .
C21 C20 H20 125.2 . .
N19 C20 H20 125.2 . .
N17 C21 C20 105.9(5) . .
N17 C21 H21 127.0 . .
C20 C21 H21 127.0 . .
F25 B22 F26 111.3(15) . .
F25 B22 F23 110.6(18) . .
F26 B22 F23 106.3(19) . .
F25 B22 F24 116(2) . .
F26 B22 F24 106.9(15) . .
F23 B22 F24 104.8(12) . .
F30 B27 F28 108.0(16) . .
F30 B27 F31 114.1(14) . .
F28 B27 F31 115(2) . .
F30 B27 F29 109(2) . .
F28 B27 F29 104.9(13) . .
F31 B27 F29 105.7(12) . .
N32 C33 C34 179.1(9) . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N19 2.104(4) 2
Ag1 N1 2.107(4) .
N1 C2 1.315(6) .
N1 C5 1.374(7) .
C2 N3 1.339(6) .
C2 H2 0.9500 .
N3 C4 1.373(7) .
N3 C6 1.468(6) .
C4 C5 1.355(7) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.524(8) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C12 1.392(8) .
C7 C8 1.398(8) .
C8 C9 1.401(8) .
C8 C13 1.505(8) .
C9 C10 1.399(8) .
C9 C16 1.522(8) .
C10 C11 1.397(8) .
C10 C14 1.509(8) .
C11 C12 1.395(8) .
C11 H11 0.9500 .
C12 C15 1.512(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 1.465(7) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
N17 C18 1.349(6) .
N17 C21 1.357(8) .
C18 N19 1.305(7) .
C18 H18 0.9500 .
N19 C20 1.364(7) .
N19 Ag1 2.104(4) 2
C20 C21 1.361(9) .
C20 H20 0.9500 .
C21 H21 0.9500 .
B22 F25 1.289(16) .
B22 F26 1.362(14) .
B22 F23 1.39(3) .
B22 F24 1.44(3) .
B27 F30 1.29(2) .
B27 F28 1.306(19) .
B27 F31 1.332(18) .
B27 F29 1.43(2) .
N32 C33 1.122(8) .
C33 C34 1.450(10) .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
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
C5 N1 C2 N3 0.3(6) . .
Ag1 N1 C2 N3 178.6(3) . .
N1 C2 N3 C4 -0.4(6) . .
N1 C2 N3 C6 178.4(5) . .
C2 N3 C4 C5 0.3(7) . .
C6 N3 C4 C5 -178.6(5) . .
N3 C4 C5 N1 -0.1(7) . .
C2 N1 C5 C4 -0.1(7) . .
Ag1 N1 C5 C4 -178.4(4) . .
C2 N3 C6 C7 -3.1(8) . .
C4 N3 C6 C7 175.5(5) . .
N3 C6 C7 C12 -86.1(6) . .
N3 C6 C7 C8 96.3(6) . .
C12 C7 C8 C9 -5.0(7) . .
C6 C7 C8 C9 172.6(4) . .
C12 C7 C8 C13 174.8(4) . .
C6 C7 C8 C13 -7.6(7) . .
C7 C8 C9 C10 4.2(7) . .
C13 C8 C9 C10 -175.6(4) . .
C7 C8 C9 C16 -172.5(4) . .
C13 C8 C9 C16 7.7(7) . .
C8 C9 C10 C11 -0.3(7) . .
C16 C9 C10 C11 176.5(4) . .
C8 C9 C10 C14 -179.5(5) . .
C16 C9 C10 C14 -2.8(7) . .
C9 C10 C11 C12 -3.0(7) . .
C14 C10 C11 C12 176.2(5) . .
C8 C7 C12 C11 1.7(7) . .
C6 C7 C12 C11 -175.9(4) . .
C8 C7 C12 C15 -177.5(4) . .
C6 C7 C12 C15 4.9(7) . .
C10 C11 C12 C7 2.3(7) . .
C10 C11 C12 C15 -178.4(4) . .
C10 C9 C16 N17 80.9(6) . .
C8 C9 C16 N17 -102.4(6) . .
C9 C16 N17 C18 26.7(9) . .
C9 C16 N17 C21 -160.2(6) . .
C21 N17 C18 N19 1.1(7) . .
C16 N17 C18 N19 175.1(5) . .
N17 C18 N19 C20 -1.1(8) . .
N17 C18 N19 Ag1 168.1(4) . 2
C18 N19 C20 C21 0.7(10) . .
Ag1 N19 C20 C21 -169.4(6) 2 .
C18 N17 C21 C20 -0.6(9) . .
C16 N17 C21 C20 -174.9(7) . .
N19 C20 C21 N17 -0.1(11) . .
