Influence of lower rim C-methyl group on crystal forms and metal complexation of resorcinarene bis-crown-5
Helttunen, Kaisa; Tero, Tiia-Riikka; Nissinen, Maija; CrystEngComm 17 (2015) 3667–; doi:10.1039/C5CE00311C

data_7220277
_publ_section_title
;
 Influence of lower rim C-methyl group on crystal forms and metal
 complexation of resorcinarene bis-crown-5
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3667
_journal_paper_doi               10.1039/C5CE00311C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C52 H70 Ag O15, 0.5(C2 H6 O), O, C F3 O3 S, 0.5(H2 O)'
_chemical_formula_sum            'C54 H76 Ag F3 O20 S'
_chemical_formula_weight         1242.08
_chemical_name_common
'silver C-methyl tetramethoxy resorcinarene bis-crown-5 trifluoromethanesulfonate ethanol solvate hydrate'
_chemical_name_systematic
'silver C-methyl tetramethoxy resorcinarene bis-crown-5 trifluoromethanesulfonate ethanol solvate hydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-01-05 deposited with the CCDC.
2015-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.0806(5)
_cell_length_b                   37.7868(8)
_cell_length_c                   14.1827(3)
_cell_measurement_reflns_used    10066
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.0860
_cell_measurement_theta_min      4.2000
_cell_volume                     11297.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -66.00  -10.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  125.0000 -120.0000 112

  2 omega -112.00  -20.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7426  -37.0000 -180.0000 184

  3 omega   41.00  108.00   0.5000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 134

  4 omega   54.00   90.00   0.5000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -30.0000 72

  5 omega   53.00   91.00   0.5000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 76

  6 omega   40.00   96.00   0.5000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   30.0000 112

  7 omega  102.00  166.00   0.5000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  120.0000 128
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0127136000
_diffrn_orient_matrix_UB_12      -0.0355718000
_diffrn_orient_matrix_UB_13      -0.0497086000
_diffrn_orient_matrix_UB_21      -0.0222105000
_diffrn_orient_matrix_UB_22      0.0160043000
_diffrn_orient_matrix_UB_23      -0.0942107000
_diffrn_orient_matrix_UB_31      0.0683965000
_diffrn_orient_matrix_UB_32      0.0119674000
_diffrn_orient_matrix_UB_33      -0.0212396000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26573
_diffrn_reflns_theta_full        76.65
_diffrn_reflns_theta_max         76.65
_diffrn_reflns_theta_min         3.93
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.941
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone/ethanol/dichloromethane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.684
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         11658
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1776P)^2^+28.7281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.2731
_reflns_number_gt                9433
_reflns_number_total             11658
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-Ag1
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_database_code               7220277
_reflns_odcompleteness_completeness 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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, All O(H) groups,
  All F(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O102-O101
 2.2 with sigma of 0.02
 O101-O103
 2.2 with sigma of 0.02
 C202-C201
 1.54 with sigma of 0.02
 F105-F103
 2.2 with sigma of 0.02
 F103-F104
 2.2 with sigma of 0.02
 F104-C100
 1.37 with sigma of 0.02
 F103-C100
 1.37 with sigma of 0.02
 F105-C100
 1.37 with sigma of 0.02
 O206-H20A = O206-H20B
 0.84 with sigma of 0.02
 O200-C201
 1.43 with sigma of 0.02
 O200-H200
 0.84 with sigma of 0.02
 S111-O109
 1.43 with sigma of 0.02
 O108-O109
 2.2 with sigma of 0.02
 O109-O107
 2.2 with sigma of 0.02
 F109-C106
 1.37 with sigma of 0.02
 F110-C106
 1.37 with sigma of 0.02
 F111-F109
 2.2 with sigma of 0.02
 F111-F110
 2.2 with sigma of 0.02
 F111-C106
 1.37 with sigma of 0.02
 O205-H20H = O205-H20I
 0.84 with sigma of 0.02
 O27-C36 \\sim O27-C36A
 with sigma of 0.02
 O56-C55 \\sim O56-C55A
 with sigma of 0.02
 O53-C52 \\sim O53-C52A
 with sigma of 0.02
 O50-C51 \\sim O50-C51A
 with sigma of 0.02
 C52A-C51A \\sim C52-C51
 with sigma of 0.02
3. Rigid bond restraints
 C52A, C52, C51A, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C52A \\sim C52 \\sim C51A \\sim C51: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O204) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F104) \\sim Ueq, Uanis(F103) \\sim Ueq, Uanis(F105) \\sim Ueq: with sigma
of 5 and sigma for terminal atoms of 10
Uanis(C36A) = Uanis(C36)
Uanis(O101) = Uanis(O102) = Uanis(O103)
Uanis(C52A) = Uanis(C52)
Uanis(C201) = Uanis(C202)
Uanis(F104) = Uanis(F103) = Uanis(F105)
Uanis(O109) = Uanis(O107) = Uanis(O108)
Uanis(F109) = Uanis(F110) = Uanis(F111)
5. Others
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
 Fixed Sof: C51(0.6) H51A(0.6) H51B(0.6) C51A(0.4) H51C(0.4) H51D(0.4)
 C52(0.6) H52A(0.6) H52B(0.6) C52A(0.4) H52C(0.4) H52D(0.4) H54A(0.6) H54B(0.6)
 H54C(0.4) H54D(0.4) C55(0.4) H55A(0.4) H55B(0.4) C55A(0.6) H55C(0.6) H55D(0.6)
 C201(0.5) H20C(0.5) H20D(0.5) C202(0.5) H20E(0.5) H20F(0.5) H20G(0.5)
 F103(0.5) O101(0.5) F110(0.5) F111(0.5) O108(0.5)
6.a Rotating group:
 O206(H20A,H20B)
6.b Ternary CH refined with riding coordinates:
 C7(H7), C14(H14), C21(H21), C28(H28)
6.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,
 H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C49(H49A,H49B), C51(H51A,H51B), C51A(H51C,H51D), C52(H52A,H52B), C52A(H52C,
 H52D), C54(H54A,H54B), C54(H54C,H54D), C55(H55A,H55B), C55A(H55C,H55D),
 C57(H57A,H57B), C58(H58A,H58B), C201(H20C,H20D)
6.d Me refined with riding coordinates:
 C29(H29A,H29B,H29C)
6.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26)
6.f Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C36A(H36D,H36E,H36F), C202(H20E,H20F,H20G)
;
_shelx_res_checksum              39064