#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:52:39 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229710 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/82/7048208.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_7048208
loop_
_publ_author_name
'Dalton, Hannah L.'
'Lynes, Amy D.'
'Twamley, Brendan'
'Byrne, Kevin'
'Schmitt, Wolfgang'
'Hawes, Chris S.'
'Gunnlaugsson, Thorfinnur'
_publ_section_title
;
 Exploring the reversible host-guest chemistry of a crystalline
 octanuclear Ag(i) metallosupramolecular macrocycle formed from a simple
 pyrazinylpyridine ligand.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17266
_journal_page_last               17275
_journal_paper_doi               10.1039/c8dt04583f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H28 Cu2 N8 O14 S2'
_chemical_formula_sum            'C32 H28 Cu2 N8 O14 S2'
_chemical_formula_weight         939.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                112.189(3)
_cell_angle_beta                 95.042(4)
_cell_angle_gamma                102.088(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5753(5)
_cell_length_b                   9.5924(5)
_cell_length_c                   10.1968(5)
_cell_measurement_reflns_used    4473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.435
_cell_measurement_theta_min      4.766
_cell_volume                     833.44(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX 3 (Bruker, 2016) '
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8144
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.479
_diffrn_reflns_theta_min         4.765
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.529
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0934 before and 0.0655 after correction. The Ratio of minimum to maximum transmission is 0.6572. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             478
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0619
_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)+(0.1240P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2673
_reflns_number_total             3028
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04583f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048201--7048212.cif.'
_cod_database_code               7048208
_shelx_shelxl_version_number     2014/7
_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_max   0.843
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
 C16-H1
 1.900684 with sigma of 0.02
 Cu1-H1
 2.630102 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
  C15(H15)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Cu1 Cu 0.24635(4) 0.52399(5) 0.60901(4) 0.0254(2) Uani 1 1 d D
S1 S -0.07437(7) 0.31341(8) 0.54339(8) 0.0263(2) Uani 1 1 d .
O1 O 0.1834(3) 0.5795(3) 0.8253(3) 0.0385(6) Uani 1 1 d D
H1 H 0.0897(13) 0.537(6) 0.807(2) 0.058 Uiso 1 1 d DR
O2 O 0.0668(2) 0.3701(3) 0.5039(2) 0.0281(5) Uani 1 1 d .
O3 O -0.0899(2) 0.1553(3) 0.5295(3) 0.0358(5) Uani 1 1 d .
O4 O -0.1940(2) 0.3127(3) 0.4385(3) 0.0314(5) Uani 1 1 d .
O5 O -0.0812(2) 0.4200(3) 0.6898(3) 0.0352(5) Uani 1 1 d .
O6 O 1.4323(3) 1.1092(3) 0.9453(3) 0.0373(6) Uani 1 1 d .
O7 O 1.3663(3) 1.3075(3) 0.9337(3) 0.0381(6) Uani 1 1 d .
N1 N 0.4505(3) 0.6561(3) 0.6802(3) 0.0261(5) Uani 1 1 d .
N2 N 0.3488(3) 0.3609(3) 0.6171(3) 0.0258(5) Uani 1 1 d .
N3 N 0.5150(3) 0.1668(3) 0.6481(3) 0.0304(6) Uani 1 1 d .
N4 N 1.3393(3) 1.1714(3) 0.9201(3) 0.0320(6) Uani 1 1 d .
C1 C 0.2873(3) 0.2117(4) 0.5852(3) 0.0286(6) Uani 1 1 d .
H1A H 0.1852 0.1712 0.5527 0.034 Uiso 1 1 calc R
C2 C 0.3714(3) 0.1142(4) 0.5991(4) 0.0307(6) Uani 1 1 d .
H2 H 0.3256 0.0071 0.5730 0.037 Uiso 1 1 calc R
C3 C 0.5749(3) 0.3172(4) 0.6797(3) 0.0289(6) Uani 1 1 d .
H3 H 0.6766 0.3582 0.7143 0.035 Uiso 1 1 calc R
C4 C 0.4934(3) 0.4156(4) 0.6637(3) 0.0266(6) Uani 1 1 d .
C5 C 0.5528(3) 0.5821(4) 0.6930(3) 0.0263(6) Uani 1 1 d .
C6 C 0.7010(3) 0.6587(4) 0.7272(3) 0.0266(6) Uani 1 1 d .
H6 H 0.7713 0.6035 0.7325 0.032 Uiso 1 1 calc R
C7 C 0.7453(3) 0.8170(4) 0.7535(3) 0.0273(6) Uani 1 1 d .
C8 C 0.6347(3) 0.8913(4) 0.7451(3) 0.0298(6) Uani 1 1 d .
H8 H 0.6591 0.9995 0.7656 0.036 Uiso 1 1 calc R
C9 C 0.4920(3) 0.8074(4) 0.7075(3) 0.0295(7) Uani 1 1 d .
H9 H 0.4194 0.8595 0.7004 0.035 Uiso 1 1 calc R
C10 C 0.9004(3) 0.9053(4) 0.7904(3) 0.0287(6) Uani 1 1 d .
C11 C 1.0091(3) 0.8466(4) 0.8353(3) 0.0278(6) Uani 1 1 d .
H11 H 0.9834 0.7467 0.8380 0.033 Uiso 1 1 calc R
C12 C 1.1526(3) 0.9313(4) 0.8755(3) 0.0296(6) Uani 1 1 d .
H12 H 1.2258 0.8906 0.9051 0.036 Uiso 1 1 calc R
C13 C 1.1878(3) 1.0771(4) 0.8718(3) 0.0298(6) Uani 1 1 d .
C14 C 1.0840(4) 1.1378(4) 0.8236(3) 0.0313(7) Uani 1 1 d .
H14 H 1.1108 1.2374 0.8205 0.038 Uiso 1 1 calc R
C15 C 0.9415(3) 1.0497(4) 0.7807(3) 0.0303(7) Uani 1 1 d .
H15 H 0.8700 1.0875 0.7439 0.036 Uiso 1 1 calc R
C16 C 0.2348(4) 0.6105(4) 0.9712(4) 0.0396(8) Uani 1 1 d D
H16A H 0.2052 0.5147 0.9868 0.059 Uiso 1 1 calc GR
H16B H 0.1936 0.6905 1.0349 0.059 Uiso 1 1 calc GR
H16C H 0.3411 0.6478 0.9927 0.059 Uiso 1 1 calc GR
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'
Cu Cu -1.9646 0.5888 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
O2 Cu1 O1 95.14(9) . .
O2 Cu1 O4 94.28(9) . 2_566
O2 Cu1 N1 167.08(10) . .
O2 Cu1 N2 93.03(10) . .
O4 Cu1 O1 100.78(10) 2_566 .
O4 Cu1 N1 89.08(10) 2_566 .
O4 Cu1 N2 161.32(11) 2_566 .
N1 Cu1 O1 96.48(10) . .
N1 Cu1 N2 80.23(10) . .
N2 Cu1 O1 95.64(10) . .
O3 S1 O2 109.26(13) . .
O3 S1 O4 108.19(14) . .
O3 S1 O5 112.49(15) . .
O4 S1 O2 107.83(13) . .
O5 S1 O2 109.78(13) . .
O5 S1 O4 109.18(13) . .
Cu1 O1 H1 104.7(13) . .
C16 O1 Cu1 143.8(2) . .
C16 O1 H1 107.4(13) . .
S1 O2 Cu1 134.56(14) . .
S1 O4 Cu1 133.16(14) . 2_566
C5 N1 Cu1 116.2(2) . .
C9 N1 Cu1 124.8(2) . .
C9 N1 C5 118.9(3) . .
C1 N2 Cu1 126.9(2) . .
C1 N2 C4 118.6(3) . .
C4 N2 Cu1 114.5(2) . .
C3 N3 C2 116.7(3) . .
O6 N4 C13 117.8(3) . .
O7 N4 O6 123.7(3) . .
O7 N4 C13 118.5(3) . .
N2 C1 H1A 119.8 . .
N2 C1 C2 120.4(3) . .
C2 C1 H1A 119.8 . .
N3 C2 C1 122.0(3) . .
N3 C2 H2 119.0 . .
C1 C2 H2 119.0 . .
N3 C3 H3 118.9 . .
N3 C3 C4 122.2(3) . .
C4 C3 H3 118.9 . .
N2 C4 C3 120.0(3) . .
N2 C4 C5 114.8(3) . .
C3 C4 C5 125.2(3) . .
N1 C5 C4 113.9(3) . .
N1 C5 C6 121.4(3) . .
C6 C5 C4 124.6(3) . .
C5 C6 H6 120.1 . .
C5 C6 C7 119.9(3) . .
C7 C6 H6 120.1 . .
C6 C7 C8 116.8(3) . .
C6 C7 C10 122.6(3) . .
C8 C7 C10 120.6(3) . .
C7 C8 H8 120.0 . .
C9 C8 C7 120.0(3) . .
C9 C8 H8 120.0 . .
N1 C9 C8 123.0(3) . .
N1 C9 H9 118.5 . .
C8 C9 H9 118.5 . .
C11 C10 C7 121.0(3) . .
C11 C10 C15 118.5(3) . .
C15 C10 C7 120.5(3) . .
C10 C11 H11 119.4 . .
C12 C11 C10 121.2(3) . .
C12 C11 H11 119.4 . .
C11 C12 H12 120.7 . .
C11 C12 C13 118.6(3) . .
C13 C12 H12 120.7 . .
C12 C13 N4 119.2(3) . .
C12 C13 C14 122.2(3) . .
C14 C13 N4 118.7(3) . .
C13 C14 H14 120.8 . .
C15 C14 C13 118.4(3) . .
C15 C14 H14 120.8 . .
C10 C15 H15 119.5 . .
C14 C15 C10 121.0(3) . .
C14 C15 H15 119.5 . .
O1 C16 H16A 109.5 . .
O1 C16 H16B 109.5 . .
O1 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.235(2) .
Cu1 O2 1.924(2) .
Cu1 O4 1.949(2) 2_566
Cu1 N1 1.993(3) .
Cu1 N2 2.035(3) .
S1 O2 1.495(2) .
S1 O3 1.442(2) .
S1 O4 1.494(2) .
S1 O5 1.473(3) .
O1 H1 0.874(10) .
O1 C16 1.421(4) .
O4 Cu1 1.949(2) 2_566
O6 N4 1.230(4) .
O7 N4 1.228(4) .
N1 C5 1.349(4) .
N1 C9 1.333(4) .
N2 C1 1.327(4) .
N2 C4 1.346(4) .
N3 C2 1.339(4) .
N3 C3 1.336(4) .
N4 C13 1.467(4) .
C1 H1A 0.9500 .
C1 C2 1.393(5) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C3 C4 1.389(5) .
C4 C5 1.480(4) .
C5 C6 1.399(4) .
C6 H6 0.9500 .
C6 C7 1.400(5) .
C7 C8 1.408(4) .
C7 C10 1.483(4) .
C8 H8 0.9500 .
C8 C9 1.369(5) .
C9 H9 0.9500 .
C10 C11 1.402(4) .
C10 C15 1.402(5) .
C11 H11 0.9500 .
C11 C12 1.377(5) .
C12 H12 0.9500 .
C12 C13 1.383(5) .
C13 C14 1.393(5) .
C14 H14 0.9500 .
C14 C15 1.378(5) .
C15 H15 0.9500 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
