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_7220274
_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, 3(C H Cl3)'
_chemical_formula_sum            'C55 H71 Cl9 O14'
_chemical_formula_weight         1275.17
_chemical_name_common
;
C-methyl tetramethoxy resorcinarene bis-crown-5 chloroform solvate
;
_chemical_name_systematic
'C-methyl tetramethoxy resorcinarene bis-crown-5 chloroform solvate'
_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_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                 108.034(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5687(4)
_cell_length_b                   23.0884(5)
_cell_length_c                   15.7904(3)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.8210
_cell_measurement_theta_min      3.2870
_cell_volume                     6090.4(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0107
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
  1 omega  -33.00   54.00   0.5000   87.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4421   57.0000  -30.0000 174

  2 omega   -3.00   84.00   0.5000   87.0000
omega____ theta____ kappa____ phi______ frames
    -       15.3015   57.0000  120.0000 174
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0381675000
_diffrn_orient_matrix_UB_12      0.0125373000
_diffrn_orient_matrix_UB_13      -0.0060041000
_diffrn_orient_matrix_UB_21      0.0167795000
_diffrn_orient_matrix_UB_22      0.0280402000
_diffrn_orient_matrix_UB_23      0.0010671000
_diffrn_orient_matrix_UB_31      -0.0079334000
_diffrn_orient_matrix_UB_32      -0.0009650000
_diffrn_orient_matrix_UB_33      -0.0468347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21409
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.69
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88190
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol/chloroform'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         11877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0860
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1263P)^2^+14.5935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2632
_reflns_number_gt                7502
_reflns_number_total             11877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-V
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_database_code               7220274
_chemical_oxdiff_formula         'C55 H71 O14 Cl9'
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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.a Ternary CH refined with riding coordinates:
 C28(H28), C21(H21), C14(H14), C7(H7), C100(H100), C101(H101), C102(H102)
2.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), C48(H48A,H48B),
 C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B),
  C57(H57A,H57B), C58(H58A,H58B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C23(H23), C26(H26), C16(H16), C19(H19), C9(H9), C12(H12)
2.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C34(H34A,
 H34B,H34C)
;
_shelx_res_checksum              2601