Inverted molecular cups: 1-D and 2-D Ag(i) coordination polymers from resorcinarene bis-thiacrowns
Helttunen, Kaisa; Nissinen, Maija; CrystEngComm 18 (2016) 4944–; doi:10.1039/C6CE00243A

data_7224197
_publ_section_title
;
 Inverted molecular cups: 1-D and 2-D Ag(i) coordination polymers from
 resorcinarene bis-thiacrowns
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4944
_journal_paper_doi               10.1039/C6CE00243A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C142 H192 Ag5 F15 O26 S8, 5.5(C2 H6 O), O'
_chemical_formula_sum            'C153 H227 Ag5 F15 O32.5 S8'
_chemical_formula_weight         3667.16
_chemical_name_common
;
n-Ag5[C-pentyl tetramethoxy resorcinarene bis-thiacrown]2[trifluoroacetate]5 ethanol solvate hydrate
;
_chemical_name_systematic
'n-Ag5[C-pentyl tetramethoxy resorcinarene bis-thiacrown]2[trifluoroacetate]5 ethanol solvate hydrate'
_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   geom
_audit_creation_date             2015-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2016-01-25 deposited with the CCDC.
2016-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                92.255(2)
_cell_angle_beta                 98.785(2)
_cell_angle_gamma                106.258(3)
_cell_formula_units_Z            2
_cell_length_a                   17.7963(6)
_cell_length_b                   20.7997(6)
_cell_length_c                   24.3087(5)
_cell_measurement_reflns_used    17752
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.0270
_cell_measurement_theta_min      3.8940
_cell_volume                     8504.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega -112.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  -57.0000 -180.0000 98

  2 omega  -70.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   57.0000  -30.0000 100

  3 omega  -93.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513  125.0000   30.0000 91

  4 omega   30.00   91.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000  -60.0000 61

  5 omega   30.00   91.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000  120.0000 61

  6 omega   24.00  101.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  -60.0000 77

  7 omega   40.00   91.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000 -120.0000 51

  8 omega   78.00  177.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   30.0000  -90.0000 99

  9 omega   52.00  122.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601 -125.0000  -90.0000 70

 10 omega   32.00   91.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000   60.0000 59

 11 omega   30.00   88.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000    0.0000 58

 12 omega   44.00  108.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000    0.0000 64

 13 omega   36.00  134.00   1.0000   47.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -77.0000   60.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0759951000
_diffrn_orient_matrix_UB_12      0.0187526000
_diffrn_orient_matrix_UB_13      0.0071545000
_diffrn_orient_matrix_UB_21      -0.0452209000
_diffrn_orient_matrix_UB_22      -0.0750541000
_diffrn_orient_matrix_UB_23      -0.0009392000
_diffrn_orient_matrix_UB_31      0.0235565000
_diffrn_orient_matrix_UB_32      0.0035453000
_diffrn_orient_matrix_UB_33      0.0639631000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52066
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.578
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             3806
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, ethanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.390
_refine_diff_density_min         -2.023
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.00028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1997
_refine_ls_number_reflns         32678
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20529
_reflns_number_total             32678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00243a2.cif
_cod_data_source_block           3-A
_cod_depositor_comments
'Adding full bibliography for 7224194--7224197.cif.'
_cod_original_cell_volume        8504.8(4)
_cod_original_formula_sum        'C153 H227 Ag5 F15 O32.50 S8'
_cod_database_code               7224197
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Shared sites
{C61, C61B}
3. Restrained distances
 F11-C74
 1.39 with sigma of 0.02
 C52A-C53A = C54A-C53A = C54A-C55A = C56A-C55A
 1.54 with sigma of 0.02
 O109-C110
 1.43 with sigma of 0.02
 C111-C110
 1.54 with sigma of 0.02
 C113-C114
 1.54 with sigma of 0.02
 C113-O112
 1.43 with sigma of 0.02
 C104-C105
 1.54 with sigma of 0.02
 O103-C104
 1.43 with sigma of 0.02
 C101-O100
 1.43 with sigma of 0.02
 C101-C102
 1.54 with sigma of 0.02
 C116-O117
 1.43 with sigma of 0.02
 C115-C116
 1.54 with sigma of 0.02
 C55B-C54A = C56A-C55B
 1.54 with sigma of 0.02
 C66A-C65A = C65A-C64A
 1.54 with sigma of 0.02
 C66B-C65A
 1.54 with sigma of 0.02
 F10-C74 = F12-C74
 1.39 with sigma of 0.02
 O106-C107
 1.43 with sigma of 0.02
 C108-C107
 1.54 with sigma of 0.02
 O109-C111
 2.42 with sigma of 0.02
 O103-C105
 2.42 with sigma of 0.02
 O100-C102
 2.42 with sigma of 0.02
 O106-C108
 2.42 with sigma of 0.02
 O112-C114
 2.42 with sigma of 0.02
 C115-O117
 2.42 with sigma of 0.02
 C59B-C60B
 1.54 with sigma of 0.02
 C58-C59B
 1.54 with sigma of 0.02
 C58-C59 = C60-C59 = C58-C57
 1.54 with sigma of 0.02
 C61-C60B = C61-C60
 1.54 with sigma of 0.02
 C61B-C60B
 1.54 with sigma of 0.02
 O1-C33 \\sim O1-C33B
 with sigma of 0.02
 C33-C34 \\sim C33B-C34
 with sigma of 0.02
4. Rigid bond restraints
 C52A, C53A, C54A, C55A, C55B, C56A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C66A, C66B, C65A, C64A, C63A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F12, F11, F10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C108, C107, O106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O100, C101, C102
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C111, C110, O109
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O112, C113, C114
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C105, C104, O103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C115, C116, O117
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C59B, C59, C60B, C60, C61, C58, C61B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C52A \\sim C53A \\sim C54A \\sim C55A \\sim C55B \\sim C56A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C66A \\sim C66B \\sim C65A \\sim C64A \\sim C63A: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
F12 \\sim F11 \\sim F10: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C108 \\sim C107 \\sim O106: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O100 \\sim C101 \\sim C102: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C111 \\sim C110 \\sim O109: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O112 \\sim C113 \\sim C114: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C105 \\sim C104 \\sim O103: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O117 \\sim C116 \\sim C115: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C61 \\sim C60 \\sim C60B \\sim C59 \\sim C59B \\sim C58 \\sim C61B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C114) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C102) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O118) \\sim Ueq, Uanis(O119) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C33B) = Uanis(C33)
Uanis(C61) = Uanis(C61B)
Uanis(C66B) = Uanis(C66A)
6. Others
 Sof(H34C)=Sof(H34D)=Sof(C33B)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H34A)=Sof(H34B)=FVAR(1)
 Sof(H54E)=Sof(H54F)=Sof(H56G)=Sof(H56H)=Sof(H56I)=Sof(C55B)=Sof(H55E)=
 Sof(H55F)=1-FVAR(2)
 Sof(H54C)=Sof(H54D)=Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(H56D)=Sof(H56E)=
 Sof(H56F)=FVAR(2)
 Sof(H58C)=Sof(H58D)=Sof(H65E)=Sof(H65F)=Sof(C59B)=Sof(H59E)=Sof(H59F)=
 Sof(C60B)=Sof(H60E)=Sof(H60F)=Sof(C61B)=Sof(H61G)=Sof(H61H)=Sof(H61I)=
 Sof(C66B)=Sof(H66G)=Sof(H66H)=Sof(H66I)=1-FVAR(3)
 Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66D)=
 Sof(H66E)=Sof(H66F)=FVAR(3)
 Fixed Sof: O117(0.5) H117(0.5) C115(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
 C116(0.5) H11D(0.5) H11E(0.5) O118(0.5) O119(0.5)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C7A(H7A), C14A(H14A), C21A(H21A),
 C28A(H28A)
7.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C34(H34C,H34D), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,
 H50B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
 C57(H57A,H57B), C58(H58A,H58B), C58(H58C,H58D), C59(H59A,H59B), C60(H60A,H60B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C33A(H33C,
 H33D), C34A(H34E,H34F), C35A(H35C,H35D), C36A(H36C,H36D), C37A(H37C,H37D),
 C38A(H38C,H38D), C39A(H39C,H39D), C40A(H40C,H40D), C41A(H41C,H41D), C42A(H42C,
 H42D), C43A(H43C,H43D), C44A(H44C,H44D), C45A(H45C,H45D), C46A(H46C,H46D),
 C47A(H47C,H47D), C48A(H48C,H48D), C49A(H49C,H49D), C50A(H50C,H50D), C52A(H52C,
 H52D), C53A(H53C,H53D), C54A(H54C,H54D), C54A(H54E,H54F), C55A(H55C,H55D),
 C57A(H57C,H57D), C58A(H58E,H58F), C59A(H59C,H59D), C60A(H60C,H60D), C62A(H62C,
 H62D), C63A(H63C,H63D), C64A(H64C,H64D), C65A(H65C,H65D), C65A(H65E,H65F),
 C33B(H33E,H33F), C55B(H55E,H55F), C59B(H59E,H59F), C60B(H60E,H60F), C107(H10A,
 H10B), C116(H11D,H11E), C110(H11F,H11G), C113(H11K,H11L), C101(H10F,H10G),
 C104(H10K,H10L)
7.c Me refined with riding coordinates:
 C61(H61A,H61B,H61C), C56A(H56D,H56E,H56F), C56A(H56G,H56H,H56I), C61A(H61D,
 H61E,H61F), C66A(H66D,H66E,H66F), C61B(H61G,H61H,H61I), C66B(H66G,H66H,H66I),
 C108(H10C,H10D,H10E), C115(H11A,H11B,H11C), C105(H10M,H10N,H10O)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C2A(H2A), C5A(H5A), C9A(H9A), C12A(H12A), C16A(H16A), C19A(H19A), C23A(H23A),
 C26A(H26A)
7.e Tetrahedral OH refined with riding coordinates:
 O106(H106), O117(H117), O109(H109), O112(H112), O100(H100), O103(H103)
7.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C66(H66A,H66B,H66C),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F), C32A(H32D,
 H32E,H32F), C51A(H51D,H51E,H51F), C111(H11H,H11I,H11J), C114(H11M,H11N,H11O),
 C102(H10H,H10I,H10J)
;
_shelx_res_checksum              3855
_olex2_submission_special_instructions 'No special instructions were received'