#------------------------------------------------------------------------------
#$Date: 2022-10-28 01:54:03 +0300 (Fri, 28 Oct 2022) $
#$Revision: 278839 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/15/7711579.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_7711579
loop_
_publ_author_name
'Tzeng, Biing-Chiau'
'Wu, Chung-Lun'
'Hung, Jun-Wei'
'Chien, Su-Ying'
'Lee, Gene-Hsiang'
_publ_section_title
;
 Supramolecular assembly and structural transformation of d10-metal
 complexes containing (aza-15-crown-5)dithiocarbamate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02768B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_sum            'C22 H40 Ag N2 O8 Rb S4'
_chemical_formula_weight         782.14
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-08-06 deposited with the CCDC.	2022-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.70500(7)
_cell_length_b                   9.70500(7)
_cell_length_c                   58.1123(7)
_cell_measurement_reflns_used    29801
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.42
_cell_volume                     4740.12(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            43051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.103
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  0.6476
_exptl_absorpt_correction_T_min  0.3633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       lath
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.023(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0266P)²+3.4071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.597
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4502
_reflns_number_total             4631
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02768b2.cif
_cod_data_source_block           ic20607
_cod_original_cell_volume        4740.12(9)
_cod_database_code               7711579
_shelx_shelxl_version_number     2018/3
_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   0.539
_shelx_estimated_absorpt_t_max   0.736
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
'y, x, -z+2/3'
'x-y, -y, -z'
'-x, -x+y, -z+1/3'
'-y, -x, -z+1/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+5/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.000000 0.76665(4) 0.666667 0.03705(10) Uani 1 2 d S T P . .
Rb1 Rb 0.85742(2) 1.14258(2) 0.583333 0.02411(9) Uani 1 2 d S T P . .
S1 S 0.19259(9) 0.93925(9) 0.63663(2) 0.02679(14) Uani 1 1 d . . . . .
S2 S 0.29050(9) 0.77795(10) 0.67099(2) 0.02806(15) Uani 1 1 d . . . . .
O1 O 0.7162(4) 0.8844(4) 0.61808(4) 0.0474(7) Uani 1 1 d . . . . .
O2 O 0.7422(3) 0.8221(3) 0.57066(4) 0.0397(6) Uani 1 1 d . . . . .
O3 O 0.6669(3) 1.0058(3) 0.54258(4) 0.0363(5) Uani 1 1 d . . . . .
O4 O 0.5441(3) 1.1143(3) 0.57906(3) 0.0312(5) Uani 1 1 d . . . . .
N1 N 0.4842(3) 0.9800(3) 0.63900(4) 0.0224(4) Uani 1 1 d . . . . .
C1 C 0.6156(4) 0.9679(5) 0.64943(5) 0.0325(7) Uani 1 1 d . . . . .
H1A H 0.595435 0.950194 0.666166 0.039 Uiso 1 1 calc R U . . .
H1B H 0.714880 1.071147 0.647420 0.039 Uiso 1 1 calc R U . . .
C2 C 0.6418(4) 0.8395(5) 0.64004(6) 0.0369(7) Uani 1 1 d . . . . .
H2A H 0.709877 0.820300 0.650724 0.044 Uiso 1 1 calc R U . . .
H2B H 0.538535 0.739615 0.638624 0.044 Uiso 1 1 calc R U . . .
C3 C 0.7741(7) 0.7849(6) 0.61004(7) 0.0587(13) Uani 1 1 d . . . . .
H3A H 0.753821 0.703182 0.621822 0.070 Uiso 1 1 calc R U . . .
H3B H 0.890611 0.849444 0.607732 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6986(6) 0.7062(5) 0.58840(8) 0.0496(10) Uani 1 1 d . . . . .
H4A H 0.732914 0.629129 0.584170 0.059 Uiso 1 1 calc R U . . .
H4B H 0.581554 0.647240 0.590275 0.059 Uiso 1 1 calc R U . . .
C5 C 0.6688(5) 0.7582(5) 0.54936(7) 0.0454(9) Uani 1 1 d . . . . .
H5A H 0.552571 0.690011 0.551502 0.055 Uiso 1 1 calc R U . . .
H5B H 0.710609 0.691961 0.542873 0.055 Uiso 1 1 calc R U . . .
C6 C 0.7023(6) 0.8911(6) 0.53325(6) 0.0478(10) Uani 1 1 d . . . . .
H6A H 0.816180 0.945300 0.528911 0.057 Uiso 1 1 calc R U . . .
H6B H 0.639018 0.846071 0.519062 0.057 Uiso 1 1 calc R U . . .
C7 C 0.4983(5) 0.9445(5) 0.54575(6) 0.0410(8) Uani 1 1 d . . . . .
H7A H 0.452829 0.848110 0.555532 0.049 Uiso 1 1 calc R U . . .
H7B H 0.443479 0.914975 0.530674 0.049 Uiso 1 1 calc R U . . .
C8 C 0.4739(5) 1.0679(5) 0.55683(6) 0.0389(8) Uani 1 1 d . . . . .
H8A H 0.519170 1.162989 0.546774 0.047 Uiso 1 1 calc R U . . .
H8B H 0.358219 1.027450 0.558178 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4666(4) 0.9961(4) 0.59652(5) 0.0280(6) Uani 1 1 d . . . . .
H9A H 0.497158 0.913104 0.595378 0.034 Uiso 1 1 calc R U . . .
H9B H 0.349568 0.945057 0.595104 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5231(3) 1.0856(4) 0.61917(5) 0.0254(6) Uani 1 1 d . . . . .
H10A H 0.639859 1.156938 0.618503 0.031 Uiso 1 1 calc R U . . .
H10B H 0.473770 1.152725 0.621223 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3368(3) 0.9047(3) 0.64815(4) 0.0221(5) 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 0.0033 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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 '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
_geom_angle_publ_flag
S1 Ag1 S1 145.44(4) 9_556 . ?
S1 Ag1 S2 130.27(2) 9_556 . ?
S1 Ag1 S2 68.39(2) . . ?
S1 Ag1 S2 68.39(2) 9_556 9_556 ?
S1 Ag1 S2 130.27(2) . 9_556 ?
S2 Ag1 S2 124.18(4) . 9_556 ?
O2 Rb1 O2 104.78(11) . 10_776 ?
O2 Rb1 O3 58.01(7) . . ?
O2 Rb1 O3 136.12(7) 10_776 . ?
O2 Rb1 O3 136.11(7) . 10_776 ?
O2 Rb1 O3 58.01(7) 10_776 10_776 ?
O3 Rb1 O3 162.00(10) . 10_776 ?
O2 Rb1 O4 161.14(7) . 10_776 ?
O2 Rb1 O4 93.08(8) 10_776 10_776 ?
O3 Rb1 O4 104.68(7) . 10_776 ?
O3 Rb1 O4 59.35(6) 10_776 10_776 ?
O2 Rb1 O4 93.08(8) . . ?
O2 Rb1 O4 161.14(7) 10_776 . ?
O3 Rb1 O4 59.35(6) . . ?
O3 Rb1 O4 104.68(7) 10_776 . ?
O4 Rb1 O4 69.96(10) 10_776 . ?
O2 Rb1 O1 96.26(9) . 10_776 ?
O2 Rb1 O1 59.10(8) 10_776 10_776 ?
O3 Rb1 O1 81.53(8) . 10_776 ?
O3 Rb1 O1 104.54(9) 10_776 10_776 ?
O4 Rb1 O1 87.65(7) 10_776 10_776 ?
O4 Rb1 O1 125.74(7) . 10_776 ?
O2 Rb1 O1 59.10(8) . . ?
O2 Rb1 O1 96.26(9) 10_776 . ?
O3 Rb1 O1 104.54(9) . . ?
O3 Rb1 O1 81.53(8) 10_776 . ?
O4 Rb1 O1 125.74(7) 10_776 . ?
O4 Rb1 O1 87.66(7) . . ?
O1 Rb1 O1 141.28(10) 10_776 . ?
O2 Rb1 C9 151.88(7) . 10_776 ?
O2 Rb1 C9 81.61(8) 10_776 10_776 ?
O3 Rb1 C9 98.17(7) . 10_776 ?
O3 Rb1 C9 70.69(7) 10_776 10_776 ?
O4 Rb1 C9 24.65(7) 10_776 10_776 ?
O4 Rb1 C9 85.46(8) . 10_776 ?
O1 Rb1 C9 63.04(8) 10_776 10_776 ?
O1 Rb1 C9 148.54(7) . 10_776 ?
O2 Rb1 C3 86.55(11) . 10_776 ?
O2 Rb1 C3 42.08(10) 10_776 10_776 ?
O3 Rb1 C3 94.33(10) . 10_776 ?
O3 Rb1 C3 97.49(11) 10_776 10_776 ?
O4 Rb1 C3 103.32(10) 10_776 10_776 ?
O4 Rb1 C3 147.87(8) . 10_776 ?
O1 Rb1 C3 23.43(8) 10_776 10_776 ?
O1 Rb1 C3 118.80(9) . 10_776 ?
C9 Rb1 C3 80.21(10) 10_776 10_776 ?
O2 Rb1 C6 118.83(9) . 10_776 ?
O2 Rb1 C6 40.86(9) 10_776 10_776 ?
O3 Rb1 C6 176.01(8) . 10_776 ?
O3 Rb1 C6 21.98(8) 10_776 10_776 ?
O4 Rb1 C6 78.78(8) 10_776 10_776 ?
O4 Rb1 C6 124.23(8) . 10_776 ?
O1 Rb1 C6 96.74(10) 10_776 10_776 ?
O1 Rb1 C6 74.55(10) . 10_776 ?
C9 Rb1 C6 84.17(9) 10_776 10_776 ?
C3 Rb1 C6 82.86(11) 10_776 10_776 ?
O2 Rb1 C10 128.98(7) . 10_776 ?
O2 Rb1 C10 98.57(8) 10_776 10_776 ?
O3 Rb1 C10 73.66(7) . 10_776 ?
O3 Rb1 C10 94.70(7) 10_776 10_776 ?
O4 Rb1 C10 39.81(6) 10_776 10_776 ?
O4 Rb1 C10 73.96(7) . 10_776 ?
O1 Rb1 C10 58.97(7) 10_776 10_776 ?
O1 Rb1 C10 159.72(7) . 10_776 ?
C9 Rb1 C10 24.52(7) 10_776 10_776 ?
C3 Rb1 C10 81.40(9) 10_776 10_776 ?
C6 Rb1 C10 108.57(9) 10_776 10_776 ?
C11 S1 Ag1 90.36(10) . . ?
C11 S2 Ag1 81.62(10) . . ?
C3 O1 C2 113.6(3) . . ?
C3 O1 Rb1 100.2(2) . . ?
C2 O1 Rb1 144.9(2) . . ?
C5 O2 C4 113.8(3) . . ?
C5 O2 Rb1 123.3(2) . . ?
C4 O2 Rb1 118.6(2) . . ?
C6 O3 C7 113.1(3) . . ?
C6 O3 Rb1 108.8(2) . . ?
C7 O3 Rb1 114.66(19) . . ?
C8 O4 C9 114.4(3) . . ?
C8 O4 Rb1 114.67(18) . . ?
C9 O4 Rb1 96.88(16) . . ?
C11 N1 C10 121.6(2) . . ?
C11 N1 C1 121.5(2) . . ?
C10 N1 C1 116.8(2) . . ?
N1 C1 C2 115.6(3) . . ?
O1 C2 C1 110.2(3) . . ?
O1 C3 C4 111.9(4) . . ?
O2 C4 C3 109.7(3) . . ?
O2 C5 C6 109.1(3) . . ?
O3 C6 C5 113.8(3) . . ?
O3 C7 C8 109.2(3) . . ?
O4 C8 C7 113.9(3) . . ?
O4 C9 C10 105.2(3) . . ?
N1 C10 C9 112.9(3) . . ?
N1 C11 S2 121.5(2) . . ?
N1 C11 S1 119.0(2) . . ?
S2 C11 S1 119.56(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 S1 2.4930(7) 9_556 ?
Ag1 S1 2.4930(7) . ?
Ag1 S2 2.7775(8) . ?
Ag1 S2 2.7775(9) 9_556 ?
Rb1 O2 2.826(3) . ?
Rb1 O2 2.826(3) 10_776 ?
Rb1 O3 2.887(2) . ?
Rb1 O3 2.887(2) 10_776 ?
Rb1 O4 2.924(2) 10_776 ?
Rb1 O4 2.924(2) . ?
Rb1 O1 2.966(3) 10_776 ?
Rb1 O1 2.967(3) . ?
Rb1 C9 3.406(3) 10_776 ?
Rb1 C3 3.508(4) 10_776 ?
Rb1 C6 3.608(4) 10_776 ?
Rb1 C10 3.657(3) 10_776 ?
S1 C11 1.728(3) . ?
S2 C11 1.710(3) . ?
O1 C3 1.418(4) . ?
O1 C2 1.423(4) . ?
O2 C5 1.408(4) . ?
O2 C4 1.425(5) . ?
O3 C6 1.426(4) . ?
O3 C7 1.447(4) . ?
O4 C8 1.424(4) . ?
O4 C9 1.431(4) . ?
N1 C11 1.348(4) . ?
N1 C10 1.461(4) . ?
N1 C1 1.469(4) . ?
C1 C2 1.494(5) . ?
C3 C4 1.463(7) . ?
C5 C6 1.492(6) . ?
C7 C8 1.479(5) . ?
C9 C10 1.520(4) . ?
