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_7224195
_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
'C62 H76 Ag3 F9 O14 S6, 5(C2 H6 O), 0.5(O H2)'
_chemical_formula_sum            'C72 H107 Ag3 F9 O19.5 S6'
_chemical_formula_weight         1971.54
_chemical_name_common
;
n-Ag3[C-ethyl tetramethoxy resorcinarene bis-thiacrown][trifluoroacetate]3 ethanol solvate hydrate
;
_chemical_name_systematic
'n-Ag3[C-ethyl tetramethoxy resorcinarene bis-thiacrown][trifluoroacetate]3 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
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-08-27
_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                67.754(3)
_cell_angle_beta                 71.544(3)
_cell_angle_gamma                88.853(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4639(3)
_cell_length_b                   17.1573(5)
_cell_length_c                   19.8936(8)
_cell_measurement_reflns_used    12267
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.9600
_cell_measurement_theta_min      4.4480
_cell_volume                     4306.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
  1 omega  -73.00   34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   77.0000    0.0000 107

  2 omega  -65.00   34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   77.0000  120.0000 99

  3 omega  -70.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6513   57.0000  -90.0000 101

  4 omega   34.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -45.0000 -120.0000 65

  5 omega   24.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -94.0000  -90.0000 84

  6 omega   35.00  136.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -61.0000  -30.0000 101

  7 omega  106.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  125.0000  -30.0000 72

  8 omega   61.00  169.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   15.0000   60.0000 108

  9 omega   31.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601  -30.0000   90.0000 60

 10 omega   82.00  172.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601   30.0000  120.0000 90

 11 omega   33.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6601 -125.0000 -180.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0467315000
_diffrn_orient_matrix_UB_12      0.0895361000
_diffrn_orient_matrix_UB_13      -0.0206585000
_diffrn_orient_matrix_UB_21      0.0249502000
_diffrn_orient_matrix_UB_22      0.0189035000
_diffrn_orient_matrix_UB_23      -0.0862940000
_diffrn_orient_matrix_UB_31      -0.0998351000
_diffrn_orient_matrix_UB_32      0.0340654000
_diffrn_orient_matrix_UB_33      0.0023179000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26379
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.242
_diffrn_reflns_theta_min         3.975
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             2026
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, ethanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.154
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         16614
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0856
_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/[\s^2^(Fo^2^)+(0.1727P)^2^+7.8548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13182
_reflns_number_total             16614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00243a2.cif
_cod_data_source_block           1-C
_cod_depositor_comments
'Adding full bibliography for 7224194--7224197.cif.'
_cod_original_formula_sum        'C72 H107 Ag3 F9 O19.50 S6'
_cod_database_code               7224195
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.73
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C62-C61
 1.54 with sigma of 0.02
 F7-C62 = F8-C62 = F9-C62
 1.39 with sigma of 0.02
 F7-F8
 2.27 with sigma of 0.02
 F7-F9
 2.27 with sigma of 0.02
 F9-F8
 2.27 with sigma of 0.02
 F9B-F7B
 2.27 with sigma of 0.02
 O9-C57 = O10-C57
 1.2 with sigma of 0.02
 C57-C58
 1.54 with sigma of 0.02
 F2-C58 = F3-C58 = F1-C58
 1.39 with sigma of 0.02
 F3-F2
 2.27 with sigma of 0.02
 F3-F1
 2.27 with sigma of 0.02
 F2-F1
 2.27 with sigma of 0.02
 O14-C61 = O13-C61 = O14B-C61B = O13B-C61B
 1.2 with sigma of 0.02
 F8B-F7B
 2.27 with sigma of 0.02
 F8B-F9B
 2.27 with sigma of 0.02
 C61B-C62B
 1.54 with sigma of 0.02
 F9B-C62B
 1.39 with sigma of 0.02
 F7B-C62B
 1.39 with sigma of 0.02
 F8B-C62B
 1.39 with sigma of 0.02
 O13B-C62B
 2.3 with sigma of 0.02
 O103-C104
 1.43 with sigma of 0.02
 C104-C105
 1.54 with sigma of 0.02
 O103-C105
 2.42 with sigma of 0.02
 C108-C107
 1.54 with sigma of 0.02
 O106-C107
 1.43 with sigma of 0.02
 C110-O109
 1.54 with sigma of 0.02
 O109-C110
 1.43 with sigma of 0.02
 C110-C111
 1.43 with sigma of 0.02
 C110-C111
 1.54 with sigma of 0.02
 O109-C111
 2.42 with sigma of 0.02
 O112-C113
 1.43 with sigma of 0.02
 C114-C113
 1.54 with sigma of 0.02
 O115-C116
 1.43 with sigma of 0.02
 C117-C116
 1.54 with sigma of 0.02
 O115-C117
 2.42 with sigma of 0.02
 O5-C41 \\sim O5-C41B
 with sigma of 0.02
 C42B-C41B \\sim C42-C41
 with sigma of 0.02
 S4-C42B \\sim S4-C42
 with sigma of 0.02
3. Rigid bond restraints
 O119
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, F8, F9, C62, C61, O13, O14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61B, C62B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41B, C41, C42, C42B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C102, C101, O100
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3, C58, F1, F2, C57, O10
 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
 C108, C107, O106
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O109, C110, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O109, C110, C111
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C113, C114, O112
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C117, C116, O115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O119: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
F7 \\sim F8 \\sim F9 \\sim C62 \\sim C61 \\sim O13 \\sim O14: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C41 \\sim C41B \\sim C42 \\sim C42B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C101 \\sim C102 \\sim O100: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C57 \\sim F3 \\sim C58 \\sim F1 \\sim F2 \\sim O10: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
C61B \\sim C62B: 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
C108 \\sim C107 \\sim O106: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O109 \\sim C110 \\sim C111: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O109 \\sim C110 \\sim C111: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C113 \\sim C114 \\sim O112: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C117 \\sim O115 \\sim C116: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(F9B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F7B) = Uanis(F9B) = Uanis(F8B)
5. Others
 Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=1-FVAR(1)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=FVAR(1)
 Fixed Sof: F7(0.6) F8(0.6) F9(0.6) O13(0.6) O14(0.6) C61(0.6) C62(0.6)
 F7B(0.4) F8B(0.4) F9B(0.4) O13B(0.4) O14B(0.4) C61B(0.4) C62B(0.4) O109(0.6)
 H109(0.6) C110(0.6) H11A(0.6) H11B(0.6) C111(0.6) H11C(0.6) H11D(0.6)
 H11E(0.6) O112(0.4) H112(0.4) C113(0.4) H11F(0.4) H11G(0.4) C114(0.4)
 H11H(0.4) H11I(0.4) H11J(0.4) O119(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), 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), C51(H51A,H51B), C53(H53A,
 H53B), C55(H55A,H55B), C41B(H41C,H41D), C42B(H42C,H42D), C110(H11A,H11B),
 C107(H10A,H10B), C101(H10F,H10G), C113(H11F,H11G), C104(H10K,H10L), C116(H11K,
 H11L)
6.c Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C114(H11H,H11I,H11J), C105(H10M,H10N,H10O), C117(H11M,
 H11N,H11O)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26)
6.e Tetrahedral OH refined with riding coordinates:
 O109(H109), O106(H106), O100(H100), O112(H112), O103(H103), O115(H115)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C),
 C111(H11C,H11D,H11E), C108(H10C,H10D,H10E), C102(H10H,H10I,H10J)
;
_shelx_res_checksum              7633
_olex2_submission_special_instructions 'No special instructions were received'