#------------------------------------------------------------------------------
#$Date: 2016-02-05 00:31:12 +0200 (Fri, 05 Feb 2016) $
#$Revision: 175967 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/35/7223587.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_7223587
loop_
_publ_author_name
'Ovsyannikov, A. S.'
'Noamane, M. H.'
'Abidi, R.'
'Ferlay, S.'
'Solovieva, S. E.'
'Antipin, I. S.'
'Konovalov, A. I.'
'Kyritsakas, N.'
'Hosseini, M. W.'
_publ_section_title
;
 Molecular tectonics: dimensionality and geometry control of silver
 coordination networks based on pyrazolyl appended thiacalixarenes
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              691
_journal_paper_doi               10.1039/C5CE02310F
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C30 H36 Ag N4 S4, As F6, 3(H2 O)'
_chemical_formula_sum            'C30 H42 Ag As F6 N4 O3 S4'
_chemical_formula_weight         931.70
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-11-23 deposited with the CCDC.
2015-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.4165(8)
_cell_length_b                   24.4165(8)
_cell_length_c                   13.7457(4)
_cell_measurement_reflns_used    90000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      2.5
_cell_volume                     8194.7(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0304
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            97274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.185
_diffrn_reflns_theta_min         1.668
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.316
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0842P)²+56.3223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.850
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.997
_reflns_number_gt                5148
_reflns_number_total             6060
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce02310f1.cif
_cod_data_source_block           e3549a_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7223579--7223589.cif.
;
_cod_original_cell_volume        8194.7(6)
_cod_database_code               7223587
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-y+1/2, -x, z+3/4'
'-x, y+1/2, -z+1/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-y+1, -x+1/2, z+5/4'
'-x+1/2, y+1, -z+3/4'
'y+1, x+1/2, z+5/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ag1 Ag 0.2500 0.07813(3) 0.3750 0.0386(2) Uani 1 2 d S T P
S1 S 0.16107(6) 0.02250(6) 0.49769(12) 0.0269(3) Uani 1 1 d . . .
C1 C 0.1127(3) 0.0681(2) 0.5514(4) 0.0258(11) Uani 1 1 d . . .
C2 C 0.0672(3) 0.0888(2) 0.5030(4) 0.0252(11) Uani 1 1 d . . .
C3 C 0.0347(3) 0.1266(3) 0.5520(4) 0.0256(11) Uani 1 1 d . . .
C4 C 0.0499(3) 0.1459(3) 0.6441(4) 0.0311(13) Uani 1 1 d . . .
H4 H 0.0267 0.1713 0.6765 0.037 Uiso 1 1 calc R U .
C5 C 0.0981(3) 0.1290(3) 0.6898(5) 0.0317(13) Uani 1 1 d . . .
C6 C 0.1282(3) 0.0875(3) 0.6430(4) 0.0294(12) Uani 1 1 d . . .
H6 H 0.1596 0.0725 0.6741 0.035 Uiso 1 1 calc R U .
S2 S 0.05261(7) 0.06878(7) 0.38169(12) 0.0363(4) Uani 1 1 d . . .
C7 C 0.0702(4) 0.1338(4) 0.3235(5) 0.049(2) Uani 1 1 d . . .
H7A H 0.0529 0.1349 0.2584 0.059 Uiso 1 1 calc R U .
H7B H 0.0544 0.1640 0.3624 0.059 Uiso 1 1 calc R U .
C8 C 0.1300(4) 0.1435(4) 0.3122(5) 0.0450(19) Uani 1 1 d . . .
H8A H 0.1363 0.1828 0.2986 0.054 Uiso 1 1 calc R U .
H8B H 0.1486 0.1346 0.3743 0.054 Uiso 1 1 calc R U .
N1 N 0.1544(3) 0.1108(3) 0.2339(4) 0.0426(15) Uani 1 1 d . . .
N2 N 0.2016(2) 0.0828(3) 0.2450(4) 0.0343(12) Uani 1 1 d . . .
C9 C 0.2129(3) 0.0615(4) 0.1576(5) 0.0395(17) Uani 1 1 d . . .
H9 H 0.2443 0.0399 0.1436 0.047 Uiso 1 1 calc R U .
C10 C 0.1727(4) 0.0749(5) 0.0901(6) 0.063(3) Uani 1 1 d . . .
H10 H 0.1711 0.0650 0.0234 0.075 Uiso 1 1 calc R U .
C11 C 0.1358(4) 0.1055(5) 0.1414(6) 0.069(3) Uani 1 1 d . . .
H11 H 0.1028 0.1206 0.1165 0.083 Uiso 1 1 calc R U .
C12 C 0.1150(4) 0.1527(4) 0.7873(6) 0.0457(18) Uani 1 1 d D . .
C13 C 0.1052(5) 0.2145(4) 0.7882(8) 0.066(3) Uani 1 1 d D . .
H13A H 0.1251 0.2314 0.7341 0.099 Uiso 1 1 calc R U .
H13B H 0.1183 0.2298 0.8498 0.099 Uiso 1 1 calc R U .
H13C H 0.0660 0.2219 0.7812 0.099 Uiso 1 1 calc R U .
C14 C 0.0794(7) 0.1254(8) 0.8662(8) 0.102(5) Uani 1 1 d D . .
H14A H 0.0407 0.1331 0.8533 0.153 Uiso 1 1 calc R U .
H14B H 0.0894 0.1401 0.9302 0.153 Uiso 1 1 calc R U .
H14C H 0.0855 0.0858 0.8655 0.153 Uiso 1 1 calc R U .
C15 C 0.1745(4) 0.1420(5) 0.8125(9) 0.071(4) Uani 1 1 d D . .
H15A H 0.1823 0.1028 0.8061 0.107 Uiso 1 1 calc R U .
H15B H 0.1815 0.1536 0.8796 0.107 Uiso 1 1 calc R U .
H15C H 0.1982 0.1627 0.7682 0.107 Uiso 1 1 calc R U .
As1 As 0.7500 0.47222(4) 0.3750 0.0332(2) Uani 1 2 d S T P
F1 F 0.7591(3) 0.5152(7) 0.4622(11) 0.210(9) Uani 1 1 d . . .
F2 F 0.6807(2) 0.4727(2) 0.3947(4) 0.0537(13) Uani 1 1 d . . .
F3 F 0.7584(4) 0.4239(7) 0.4560(12) 0.200(9) Uani 1 1 d . . .
O1 O 0.2493(4) 0.2184(4) 0.2133(12) 0.137(6) Uani 1 1 d . . .
O2 O 0.0000 0.0000 0.1774(12) 0.177(12) Uani 1 2 d S T P
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'
Ag Ag -0.8971 1.1015 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 '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
N2 Ag1 N2 173.9(3) . 15_545
C3 S1 C1 109.8(3) 2_556 .
C2 C1 C6 121.6(6) . .
C2 C1 S1 123.9(5) . .
C6 C1 S1 114.0(5) . .
C1 C2 C3 117.8(5) . .
C1 C2 S2 120.7(5) . .
C3 C2 S2 121.5(5) . .
C2 C3 C4 120.7(6) . .
C2 C3 S1 125.4(5) . 4_556
C4 C3 S1 113.4(5) . 4_556
C5 C4 C3 122.0(6) . .
C5 C4 H4 119.0 . .
C3 C4 H4 119.0 . .
C4 C5 C6 116.6(6) . .
C4 C5 C12 120.8(6) . .
C6 C5 C12 122.5(6) . .
C1 C6 C5 121.0(6) . .
C1 C6 H6 119.5 . .
C5 C6 H6 119.5 . .
C2 S2 C7 97.2(4) . .
C8 C7 S2 114.5(6) . .
C8 C7 H7A 108.6 . .
S2 C7 H7A 108.6 . .
C8 C7 H7B 108.6 . .
S2 C7 H7B 108.6 . .
H7A C7 H7B 107.6 . .
N1 C8 C7 112.9(8) . .
N1 C8 H8A 109.0 . .
C7 C8 H8A 109.0 . .
N1 C8 H8B 109.0 . .
C7 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
N2 N1 C11 110.1(6) . .
N2 N1 C8 122.7(6) . .
C11 N1 C8 127.1(7) . .
C9 N2 N1 105.8(6) . .
C9 N2 Ag1 127.8(5) . .
N1 N2 Ag1 126.3(5) . .
N2 C9 C10 111.1(7) . .
N2 C9 H9 124.4 . .
C10 C9 H9 124.4 . .
C11 C10 C9 104.5(7) . .
C11 C10 H10 127.8 . .
C9 C10 H10 127.8 . .
N1 C11 C10 108.4(7) . .
N1 C11 H11 125.8 . .
C10 C11 H11 125.8 . .
C5 C12 C15 113.3(7) . .
C5 C12 C13 110.0(7) . .
C15 C12 C13 108.5(8) . .
C5 C12 C14 107.7(7) . .
C15 C12 C14 107.8(10) . .
C13 C12 C14 109.4(10) . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 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 . .
F1 As1 F1 98.6(15) . 15_645
F1 As1 F3 86.9(10) . .
F1 As1 F3 174.5(11) 15_645 .
F1 As1 F3 174.5(11) . 15_645
F1 As1 F3 86.9(10) 15_645 15_645
F3 As1 F3 87.6(15) . 15_645
F1 As1 F2 90.9(3) . .
F1 As1 F2 88.6(3) 15_645 .
F3 As1 F2 91.2(4) . .
F3 As1 F2 89.4(4) 15_645 .
F1 As1 F2 88.6(3) . 15_645
F1 As1 F2 90.9(3) 15_645 15_645
F3 As1 F2 89.4(4) . 15_645
F3 As1 F2 91.2(4) 15_645 15_645
F2 As1 F2 179.2(4) . 15_645
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.146(6) .
Ag1 N2 2.146(6) 15_545
S1 C3 1.769(7) 2_556
S1 C1 1.782(6) .
C1 C2 1.390(9) .
C1 C6 1.398(8) .
C2 C3 1.391(9) .
C2 S2 1.774(6) .
C3 C4 1.402(8) .
C3 S1 1.769(7) 4_556
C4 C5 1.397(10) .
C4 H4 0.9500 .
C5 C6 1.407(10) .
C5 C12 1.516(9) .
C6 H6 0.9500 .
S2 C7 1.828(10) .
C7 C8 1.488(14) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 N1 1.467(9) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
N1 N2 1.346(8) .
N1 C11 1.357(10) .
N2 C9 1.338(9) .
C9 C10 1.390(11) .
C9 H9 0.9500 .
C10 C11 1.366(12) .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 C15 1.517(12) .
C12 C13 1.527(12) .
C12 C14 1.542(14) .
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 .
As1 F1 1.608(8) .
As1 F1 1.608(8) 15_645
As1 F3 1.635(9) .
As1 F3 1.635(9) 15_645
As1 F2 1.714(5) .
As1 F2 1.714(5) 15_645
