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_7220270
_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 O14'
_chemical_formula_sum            'C52 H68 O14'
_chemical_formula_weight         917.06
_chemical_name_common
;
C-methyl tetramethoxy resorcinarene bis-crown-5
;
_chemical_name_systematic
'C-methyl tetramethoxy resorcinarene bis-crown-5'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_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                 90.0740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.02090(10)
_cell_length_b                   16.0930(2)
_cell_length_c                   26.6261(4)
_cell_measurement_reflns_used    10519
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.2974
_cell_measurement_theta_min      3.2061
_cell_volume                     4722.38(10)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6959  125.0000 -180.0000 188

  2 omega  -49.00   30.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.6959   37.0000  120.0000 158

  3 omega -124.00  -80.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000    0.0000 88

  4 omega -114.00  -19.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -45.0000  -30.0000 190

  5 omega   90.00  176.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406   45.0000  -90.0000 172

  6 omega   32.00   91.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000    0.0000 118

  7 omega   87.00  178.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406   30.0000 -180.0000 182

  8 omega   35.00  122.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406 -125.0000  -30.0000 174

  9 omega   32.00   91.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -30.0000  150.0000 118

 10 omega   25.00  109.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -94.0000   30.0000 168

 11 omega   95.00  176.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  125.0000   90.0000 162

 12 omega   35.00  135.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.7406  -77.0000  120.0000 200
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28596
_diffrn_reflns_theta_full        74.47
_diffrn_reflns_theta_max         74.47
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56977
_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            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1-Propanol'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+2.1758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                7976
_reflns_number_total             9459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-I
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_database_code               7220270
_shelx_res_checksum              4506