#------------------------------------------------------------------------------
#$Date: 2023-12-22 17:07:40 +0200 (Fri, 22 Dec 2023) $
#$Revision: 288505 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/21/57/7215705.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_7215705
loop_
_publ_author_name
'du Plessis, Marike'
'Smith, Vincent J.'
'Barbour, Leonard J.'
_publ_section_title
;
 Single-crystal to single-crystal guest exchange and phase transformations
 in a porous metallocycle
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              4126
_journal_paper_doi               10.1039/c4ce00244j
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C32 H36 Ag2 N8, C6 H4 F2, 2(B F4)'
_chemical_formula_sum            'C38 H40 Ag2 B2 F10 N8'
_chemical_formula_weight         1036.14
_chemical_name_common            'Difluorobenzene Solvate'
_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
_cell_angle_alpha                71.505(2)
_cell_angle_beta                 89.185(2)
_cell_angle_gamma                89.430(2)
_cell_formula_units_Z            1
_cell_length_a                   7.0814(11)
_cell_length_b                   12.445(2)
_cell_length_c                   12.837(2)
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.76
_cell_volume                     1072.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'X-Seed (Barbour,2001;Atwood & Barbour,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15820
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.74
_diffrn_reflns_theta_min         1.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.9071
_exptl_absorpt_correction_T_min  0.8816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Symmetry-related measurements'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6139
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0384P)²+2.9671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                5607
_reflns_number_total             6139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00244j2.cif
_cod_data_source_block           C:
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7215705
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_group
Ag1 Ag 0.00575(3) 0.18162(2) 0.18917(2) 0.01909(8) Uani 1 1 d . .
N1 N 0.0897(4) 0.0441(2) 0.3216(2) 0.0191(5) Uani 1 1 d . .
F2 F 0.5538(3) 0.41652(18) 0.26382(19) 0.0279(5) Uani 1 1 d . .
C3 C 0.2716(5) 0.0210(3) 0.3614(3) 0.0233(7) Uani 1 1 d . .
H3 H 0.3773 0.0694 0.3371 0.028 Uiso 1 1 calc R .
C4 C 0.2750(5) -0.0816(3) 0.4406(3) 0.0252(7) Uani 1 1 d . .
H4 H 0.3812 -0.1177 0.4819 0.030 Uiso 1 1 calc R .
F3 F 0.6487(3) 0.23279(19) 0.29515(17) 0.0271(4) Uani 1 1 d . .
N2 N 0.0928(4) -0.1230(2) 0.4493(2) 0.0177(5) Uani 1 1 d . .
F4 F 0.4287(3) 0.2744(2) 0.40663(19) 0.0336(5) Uani 1 1 d . .
C2 C -0.0146(4) -0.0448(3) 0.3762(3) 0.0178(6) Uani 1 1 d . .
C1 C -0.2189(5) -0.0596(3) 0.3591(3) 0.0276(7) Uani 1 1 d . .
H1A H -0.2753 0.0141 0.3195 0.041 Uiso 1 1 calc R .
H1B H -0.2826 -0.0911 0.4305 0.041 Uiso 1 1 calc R .
H1C H -0.2335 -0.1114 0.3161 0.041 Uiso 1 1 calc R .
F1 F 0.3561(3) 0.29039(18) 0.2293(2) 0.0318(5) Uani 1 1 d . .
C5 C 0.0355(5) -0.2381(3) 0.5147(3) 0.0205(6) Uani 1 1 d . .
H5A H -0.0912 -0.2357 0.5475 0.025 Uiso 1 1 calc R .
H5B H 0.1258 -0.2695 0.5751 0.025 Uiso 1 1 calc R .
C6 C 0.0310(4) -0.3139(3) 0.4422(3) 0.0171(6) Uani 1 1 d . .
C7 C 0.1966(5) -0.3357(3) 0.3916(3) 0.0261(7) Uani 1 1 d . .
H7 H 0.3130 -0.3054 0.4050 0.031 Uiso 1 1 calc R .
C8 C 0.1927(5) -0.4009(3) 0.3221(3) 0.0255(7) Uani 1 1 d . .
H8 H 0.3066 -0.4156 0.2889 0.031 Uiso 1 1 calc R .
C9 C 0.0226(4) -0.4455(3) 0.3004(3) 0.0170(6) Uani 1 1 d . .
C15 C -0.1413(5) -0.4255(3) 0.3528(3) 0.0210(6) Uani 1 1 d . .
H15 H -0.2575 -0.4569 0.3407 0.025 Uiso 1 1 calc R .
C16 C -0.1370(5) -0.3602(3) 0.4227(3) 0.0213(6) Uani 1 1 d . .
H16 H -0.2503 -0.3471 0.4574 0.026 Uiso 1 1 calc R .
C10 C 0.0178(5) -0.5129(3) 0.2217(3) 0.0182(6) Uani 1 1 d . .
H10A H 0.1023 -0.5796 0.2483 0.022 Uiso 1 1 calc R .
H10B H -0.1121 -0.5408 0.2193 0.022 Uiso 1 1 calc R .
N3 N 0.0772(4) -0.4449(2) 0.1106(2) 0.0168(5) Uani 1 1 d . .
C11 C 0.2581(5) -0.4414(3) 0.0688(3) 0.0206(6) Uani 1 1 d . .
H11 H 0.3625 -0.4869 0.1029 0.025 Uiso 1 1 calc R .
C12 C 0.2573(5) -0.3596(3) -0.0317(3) 0.0219(6) Uani 1 1 d . .
H12 H 0.3626 -0.3382 -0.0803 0.026 Uiso 1 1 calc R .
N4 N 0.0780(4) -0.3131(2) -0.0510(2) 0.0186(5) Uani 1 1 d . .
C13 C -0.0274(4) -0.3660(3) 0.0371(3) 0.0178(6) Uani 1 1 d . .
C14 C -0.2301(5) -0.3418(3) 0.0542(3) 0.0262(7) Uani 1 1 d . .
H14A H -0.2397 -0.2958 0.1034 0.039 Uiso 1 1 calc R .
H14B H -0.2973 -0.4134 0.0870 0.039 Uiso 1 1 calc R .
H14C H -0.2866 -0.3005 -0.0167 0.039 Uiso 1 1 calc R .
B1 B 0.4967(5) 0.3039(3) 0.2996(3) 0.0182(7) Uani 1 1 d . .
C17 C 0.422(3) -0.0449(16) 0.1054(13) 0.041(6) Uiso 0.170(5) 1 d PD 2
H17 H 0.3708 -0.0734 0.1777 0.049 Uiso 0.170(5) 1 calc PR 2
C18 C 0.412(3) -0.1055(14) 0.0333(15) 0.035(5) Uiso 0.170(5) 1 d PD 2
H18 H 0.3528 -0.1774 0.0533 0.042 Uiso 0.170(5) 1 calc PR 2
C19 C 0.492(4) -0.0588(15) -0.0687(14) 0.041(6) Uiso 0.170(5) 1 d PD 2
F5 F 0.480(3) -0.1258(15) -0.1375(14) 0.055(5) Uiso 0.170(5) 1 d PD 2
C20 C -0.1666(12) 0.0500(7) -0.0474(6) 0.116(5) Uani 0.830(5) 1 d PD 1
H20 H -0.2850 0.0802 -0.0773 0.140 Uiso 0.830(5) 1 calc PR 1
C21 C -0.0012(10) 0.0913(6) -0.1010(6) 0.067(2) Uani 0.830(5) 1 d PD 1
H21 H 0.0032 0.1530 -0.1676 0.081 Uiso 0.830(5) 1 calc PR 1
C22 C 0.1571(8) 0.0361(7) -0.0505(6) 0.076(2) Uani 0.830(5) 1 d PD 1
F6 F 0.3245(8) 0.0872(7) -0.1011(6) 0.130(3) Uani 0.830(5) 1 d PD 1
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
N1 Ag1 N4 176.66(11) . 2
C2 N1 C3 106.5(3) . .
C2 N1 Ag1 126.9(2) . .
C3 N1 Ag1 126.2(2) . .
C4 C3 N1 109.2(3) . .
C4 C3 H3 125.4 . .
N1 C3 H3 125.4 . .
C3 C4 N2 106.3(3) . .
C3 C4 H4 126.8 . .
N2 C4 H4 126.8 . .
C2 N2 C4 107.7(3) . .
C2 N2 C5 126.5(3) . .
C4 N2 C5 125.2(3) . .
N1 C2 N2 110.3(3) . .
N1 C2 C1 125.8(3) . .
N2 C2 C1 123.9(3) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N2 C5 C6 109.9(3) . .
N2 C5 H5A 109.7 . .
C6 C5 H5A 109.7 . .
N2 C5 H5B 109.7 . .
C6 C5 H5B 109.7 . .
H5A C5 H5B 108.2 . .
C16 C6 C7 118.7(3) . .
C16 C6 C5 121.0(3) . .
C7 C6 C5 120.2(3) . .
C8 C7 C6 120.7(3) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C7 C8 C9 120.7(3) . .
C7 C8 H8 119.7 . .
C9 C8 H8 119.7 . .
C15 C9 C8 118.4(3) . .
C15 C9 C10 121.1(3) . .
C8 C9 C10 120.5(3) . .
C16 C15 C9 120.8(3) . .
C16 C15 H15 119.6 . .
C9 C15 H15 119.6 . .
C6 C16 C15 120.7(3) . .
C6 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
N3 C10 C9 111.6(2) . .
N3 C10 H10A 109.3 . .
C9 C10 H10A 109.3 . .
N3 C10 H10B 109.3 . .
C9 C10 H10B 109.3 . .
H10A C10 H10B 108.0 . .
C13 N3 C11 108.2(3) . .
C13 N3 C10 126.4(3) . .
C11 N3 C10 125.0(3) . .
C12 C11 N3 106.3(3) . .
C12 C11 H11 126.9 . .
N3 C11 H11 126.9 . .
C11 C12 N4 108.8(3) . .
C11 C12 H12 125.6 . .
N4 C12 H12 125.6 . .
C13 N4 C12 106.8(3) . .
C13 N4 Ag1 127.2(2) . 2
C12 N4 Ag1 126.0(2) . 2
N4 C13 N3 110.0(3) . .
N4 C13 C14 125.8(3) . .
N3 C13 C14 124.2(3) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
F4 B1 F2 110.4(3) . .
F4 B1 F3 108.9(3) . .
F2 B1 F3 110.2(3) . .
F4 B1 F1 110.4(3) . .
F2 B1 F1 108.4(3) . .
F3 B1 F1 108.5(3) . .
C19 C17 C18 117.1(14) 2_655 .
C19 C17 H17 121.4 2_655 .
C18 C17 H17 121.4 . .
C19 C18 C17 117.5(14) . .
C19 C18 H18 121.2 . .
C17 C18 H18 121.2 . .
C18 C19 C17 125.3(12) . 2_655
C18 C19 F5 114.5(16) . .
C17 C19 F5 120.2(17) 2_655 .
C21 C20 C22 118.3(8) . 2
C21 C20 H20 120.8 . .
C22 C20 H20 120.8 2 .
C22 C21 C20 114.1(7) . .
C22 C21 H21 122.9 . .
C20 C21 H21 122.9 . .
C21 C22 C20 127.5(6) . 2
C21 C22 F6 112.8(7) . .
C20 C22 F6 119.1(7) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.082(3) .
Ag1 N4 2.084(3) 2
N1 C2 1.331(4) .
N1 C3 1.386(4) .
F2 B1 1.392(4) .
C3 C4 1.356(5) .
C3 H3 0.9500 .
C4 N2 1.384(4) .
C4 H4 0.9500 .
F3 B1 1.398(4) .
N2 C2 1.353(4) .
N2 C5 1.470(4) .
F4 B1 1.386(4) .
C2 C1 1.489(5) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
F1 B1 1.399(4) .
C5 C6 1.521(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C16 1.387(4) .
C6 C7 1.398(5) .
C7 C8 1.384(5) .
C7 H7 0.9500 .
C8 C9 1.399(5) .
C8 H8 0.9500 .
C9 C15 1.393(4) .
C9 C10 1.505(4) .
C15 C16 1.389(5) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C10 N3 1.467(4) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
N3 C13 1.350(4) .
N3 C11 1.377(4) .
C11 C12 1.367(5) .
C11 H11 0.9500 .
C12 N4 1.382(4) .
C12 H12 0.9500 .
N4 C13 1.335(4) .
N4 Ag1 2.084(3) 2
C13 C14 1.491(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C17 C19 1.370(2) 2_655
C17 C18 1.370(2) .
C17 H17 0.9500 .
C18 C19 1.369(2) .
C18 H18 0.9500 .
C19 C17 1.370(2) 2_655
C19 F5 1.399(2) .
C20 C21 1.369(2) .
C20 C22 1.371(2) 2
C20 H20 0.9500 .
C21 C22 1.368(2) .
C21 H21 0.9500 .
C22 C20 1.371(2) 2
C22 F6 1.401(2) .
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
C2 N1 C3 C4 -0.5(4) . .
Ag1 N1 C3 C4 -173.7(3) . .
N1 C3 C4 N2 0.5(4) . .
C3 C4 N2 C2 -0.3(4) . .
C3 C4 N2 C5 171.6(3) . .
C3 N1 C2 N2 0.3(4) . .
Ag1 N1 C2 N2 173.4(2) . .
C3 N1 C2 C1 -178.3(3) . .
Ag1 N1 C2 C1 -5.2(5) . .
C4 N2 C2 N1 0.0(4) . .
C5 N2 C2 N1 -171.7(3) . .
C4 N2 C2 C1 178.6(3) . .
C5 N2 C2 C1 6.9(5) . .
C2 N2 C5 C6 74.8(4) . .
C4 N2 C5 C6 -95.6(4) . .
N2 C5 C6 C16 -115.5(3) . .
N2 C5 C6 C7 62.9(4) . .
C16 C6 C7 C8 0.9(5) . .
C5 C6 C7 C8 -177.5(3) . .
C6 C7 C8 C9 0.6(6) . .
C7 C8 C9 C15 -1.9(5) . .
C7 C8 C9 C10 177.8(3) . .
C8 C9 C15 C16 1.8(5) . .
C10 C9 C15 C16 -177.9(3) . .
C7 C6 C16 C15 -1.0(5) . .
C5 C6 C16 C15 177.4(3) . .
C9 C15 C16 C6 -0.3(5) . .
C15 C9 C10 N3 117.9(3) . .
C8 C9 C10 N3 -61.8(4) . .
C9 C10 N3 C13 -77.2(4) . .
C9 C10 N3 C11 94.5(4) . .
C13 N3 C11 C12 -0.7(4) . .
C10 N3 C11 C12 -173.7(3) . .
N3 C11 C12 N4 0.2(4) . .
C11 C12 N4 C13 0.3(4) . .
C11 C12 N4 Ag1 178.3(2) . 2
C12 N4 C13 N3 -0.7(4) . .
Ag1 N4 C13 N3 -178.7(2) 2 .
C12 N4 C13 C14 178.5(3) . .
Ag1 N4 C13 C14 0.6(5) 2 .
C11 N3 C13 N4 0.9(4) . .
C10 N3 C13 N4 173.8(3) . .
C11 N3 C13 C14 -178.3(3) . .
C10 N3 C13 C14 -5.4(5) . .
C19 C17 C18 C19 1(4) 2_655 .
C17 C18 C19 C17 -1(5) . 2_655
C17 C18 C19 F5 179.3(18) . .
C22 C20 C21 C22 2.7(14) 2 .
C20 C21 C22 C20 -3.0(16) . 2
C20 C21 C22 F6 -174.1(7) . .
