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_7224194
_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
'C120 H152 Ag4 F12 O24 S12, 5(C2 H6 O), 3(C H2 Cl2), 4(O)'
_chemical_formula_sum            'C135 H202 Ag4 Cl6 F12 O34 S12'
_chemical_formula_weight         3625.85
_chemical_name_common
;
n-Ag2[C-ethyl tetramethoxy resorcinarene bis-thiacrown][trifluoroacetate]2 dichloromethane ethanol solvate hydrate
;
_chemical_name_systematic
'n-Ag2[C-ethyl tetramethoxy resorcinarene bis-thiacrown][trifluoroacetate]2 dichloromethane 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             2015-08-19
_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                75.3850(7)
_cell_angle_beta                 83.6250(6)
_cell_angle_gamma                74.0640(11)
_cell_formula_units_Z            2
_cell_length_a                   18.1183(3)
_cell_length_b                   19.5986(4)
_cell_length_c                   24.7135(5)
_cell_measurement_reflns_used    16975
_cell_measurement_temperature    173
_cell_measurement_theta_max      23.225
_cell_measurement_theta_min      1.787
_cell_volume                     8157.1(3)
_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_temperature      173
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40597
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        24.000
_diffrn_reflns_theta_max         23.225
_diffrn_reflns_theta_min         1.787
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Majewski, Borek & Minor,2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             3748
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, ethanol'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1910
_refine_ls_number_reflns         22433
_refine_ls_number_restraints     208
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0952
_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^)+(0.1239P)^2^+84.0671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16975
_reflns_number_total             22433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00243a2.cif
_cod_data_source_block           1-B
_cod_depositor_comments
'Adding full bibliography for 7224194--7224197.cif.'
_cod_database_code               7224194
_shelxl_version_number           2014/6
_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 O(H) groups
2. Restrained distances
 F11-C64 = F12-C64 = F10-C64
 1.39 with sigma of 0.02
 F12B-C64 = F10B-C64
 1.39 with sigma of 0.02
 F11B-C64
 1.39 with sigma of 0.02
 F11B-F12B
 2.27 with sigma of 0.02
 F12-F11
 2.27 with sigma of 0.02
 F10-F11
 2.27 with sigma of 0.02
 F3-C58 = F2-C58 = F1-C58
 1.39 with sigma of 0.02
 F2-F1
 2.27 with sigma of 0.02
 F3-F1
 2.27 with sigma of 0.02
 F9-C62 = F8-C62 = F7-C62
 1.39 with sigma of 0.02
 F6-C60 = F4-C60 = F5-C60
 1.39 with sigma of 0.02
 F6-F4
 2.27 with sigma of 0.02
 F5-F4
 2.27 with sigma of 0.02
 F8B-C62 = F9B-C62 = F7B-C62
 1.39 with sigma of 0.02
 F7-F8
 2.27 with sigma of 0.02
 F8-F9
 2.27 with sigma of 0.02
 F7B-F8B
 2.27 with sigma of 0.02
 F8B-F9B
 2.27 with sigma of 0.02
 Cl1-C112 = Cl2-C112
 1.79 with sigma of 0.02
 Cl4-C115 = Cl3-C115
 1.79 with sigma of 0.02
 Cl6-C118 = Cl5-C118
 1.79 with sigma of 0.02
 O100-C101
 1.43 with sigma of 0.02
 C102-C101
 1.54 with sigma of 0.02
 C105-C104
 1.54 with sigma of 0.02
 O103-C104
 1.43 with sigma of 0.02
 C111-C110
 1.54 with sigma of 0.02
 O109-C110
 1.43 with sigma of 0.02
 O123-C122
 1.43 with sigma of 0.02
 C121-C122
 1.54 with sigma of 0.02
 O123-C121
 2.2 with sigma of 0.02
 Ag3-S2A \\sim Ag3-S2B
 with sigma of 0.02
 S2A-C37A \\sim S2B-C37A
 with sigma of 0.02
3. Rigid bond restraints
 F12, F10, F11, F11B, F12B, F10B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F2, F1, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F5, F6, F4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7, F7B, F8, F8B, F9, F9B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl4, Cl3, C115
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, C112, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl6, C118, Cl5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O103, C104, C105
 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
 C122, O123
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O123, C122, C121
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F12 \\sim F10B \\sim F11 \\sim F12B \\sim F11B \\sim F10: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
F3 \\sim F1 \\sim F2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F5 \\sim F6 \\sim F4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F7 \\sim F7B \\sim F8 \\sim F8B \\sim F9 \\sim F9B: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Cl4 \\sim C115 \\sim Cl3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl2 \\sim C112 \\sim Cl1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl6 \\sim C118 \\sim Cl5: 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
C111 \\sim C110 \\sim O109: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C122 \\sim O123: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O123 \\sim C122 \\sim C121: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(Ag2B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O127) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O125) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O125) \\sim Ueq, Uanis(O12B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Ag3) \\sim Ueq, Uanis(Ag3B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Ag4) = Uanis(Ag4B)
Uanis(O125) = Uanis(O12B)
5. Others
 Fixed Sof: H36C(0.75) H36D(0.75) H36E(0.25) H36F(0.25) H37C(0.75) H37D(0.75)
 H37E(0.25) H37F(0.25) Ag2B(0.1) Ag3B(0.25) Ag4B(0.1) S2B(0.25) F7B(0.25)
 F8B(0.25) F9B(0.25) Ag4(0.9) F10B(0.4) F11B(0.4) F12B(0.4) F11(0.6) S2A(0.75)
 Ag2(0.9) F10(0.6) Ag3(0.75) F12(0.6) F7(0.75) F8(0.75) F9(0.75) O125(0.5)
 O12B(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28), C7A(H7A), C14A(H14A), C21A(H21A),
 C28A(H28A)
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), C33A(H33C,H33D), C34A(H34C,H34D), C35A(H35C,H35D),
 C36A(H36C,H36D), C36A(H36E,H36F), C37A(H37C,H37D), C37A(H37E,H37F), 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), C51A(H51C,H51D), C53A(H53C,H53D),
 C55A(H55C,H55D), C122(H12E,H12F), C107(H10A,H10B), C101(H10F,H10G), C104(H10K,
 H10L), C110(H11A,H11B), C115(H11F,H11G), C112(H11H,H11I), C118(H11J,H11K)
6.c Me refined with riding coordinates:
 C121(H12B,H12C,H12D)
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),
 C2A(H2A), C5A(H5A), C9A(H9A), C12A(H12A), C16A(H16A), C19A(H19A), C23A(H23A),
 C26A(H26A)
6.e Tetrahedral OH refined with riding coordinates:
 O123(H123), O106(H106), O100(H100)
6.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C), C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F),
 C32A(H32D,H32E,H32F), C50A(H50D,H50E,H50F), C52A(H52D,H52E,H52F), C54A(H54D,
 H54E,H54F), C56A(H56D,H56E,H56F), C108(H10C,H10D,H10E), C102(H10H,H10I,H10J),
 C105(H10M,H10N,H10O), C111(H11C,H11D,H11E)
6.g Idealised tetrahedral OH refined as rotating group:
 O103(H103), O109(H109)
;
_shelx_res_checksum              4544
_olex2_submission_special_instructions 'No special instructions were received'