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_7220276
_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 H68 Ag2 O14, 2(F6 P)'
_chemical_formula_sum            'C53.5 H72.5 Ag2 F12 O15.25 P2'
_chemical_formula_weight         1465.29
_chemical_name_common
;
disilver C-methyl tetramethoxy resorcinarene bis-crown-5 di(hexafluorophosphate)
;
_chemical_name_systematic
'disilver C-methyl tetramethoxy resorcinarene bis-crown-5 di(hexafluorophosphate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-26
_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
_cell_angle_beta                 105.634(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9517(4)
_cell_length_b                   16.9799(4)
_cell_length_c                   17.9735(4)
_cell_measurement_reflns_used    4107
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.1905
_cell_measurement_theta_min      3.4708
_cell_volume                     5863.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
  1 omega -124.00  -80.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000 -180.0000 44

  2 omega  -71.00   27.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   61.0000 -150.0000 98

  3 omega  -56.00   20.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000  -30.0000 76

  4 omega   80.00  176.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      106.7406   61.0000  -90.0000 96

  5 omega   37.00  133.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -61.0000  120.0000 96

  6 omega   45.00  167.00   1.0000    3.1200
omega____ theta____ kappa____ phi______ frames
    -      106.7406    0.0000 -120.0000 122
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0267750000
_diffrn_orient_matrix_UB_12      -0.0823523000
_diffrn_orient_matrix_UB_13      0.0298136000
_diffrn_orient_matrix_UB_21      -0.0730793000
_diffrn_orient_matrix_UB_22      -0.0219616000
_diffrn_orient_matrix_UB_23      0.0067521000
_diffrn_orient_matrix_UB_31      -0.0193874000
_diffrn_orient_matrix_UB_32      -0.0311910000
_diffrn_orient_matrix_UB_33      -0.0835342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9992
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.359
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             2990
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone/1-propanol'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1199P)^2^+4.6136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4808
_reflns_number_total             5682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-Ag2
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_original_cell_volume        5863.8(2)
_cod_original_formula_sum        'C53.50 H72.50 Ag2 F12 O15.25 P2'
_cod_database_code               7220276
_shelxl_version_number           2013-4
_chemical_oxdiff_usercomment     'clear, colorless, rod'
_reflns_odcompleteness_completeness 98.68
_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
2. Restrained distances
 P1-F3 = P1-F4 = P1-F2 = P1-F5 = P1-F2A = P1-F5A
 1.57 with sigma of 0.02
 F5-F2 \\sim F4-F2 \\sim F4-F5 \\sim F3-F5 \\sim F4-F3 \\sim F5A-F2A
 with sigma of 0.02
3. Rigid bond restraints
 F2, F2A, F5, F5A, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F2 \\sim F2A \\sim F5 \\sim F5A \\sim F3: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: F2(0.3) F2A(0.2) F5(0.6) F5A(0.4)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C14(H14)
6.b 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)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C12(H12), C9(H9)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              78870