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_7220272
_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, C2 H3 N'
_chemical_formula_sum            'C54 H71 N O14'
_chemical_formula_weight         958.11
_chemical_name_common
;
C-methyl tetramethoxy resorcinarene bis-crown-5 acetonitrile solvate
;
_chemical_name_systematic
'C-methyl tetramethoxy resorcinarene bis-crown-5 acetonitrile solvate'
_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
_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                85.264(2)
_cell_angle_beta                 85.152(2)
_cell_angle_gamma                73.771(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9268(3)
_cell_length_b                   14.4126(7)
_cell_length_c                   20.6525(11)
_cell_measurement_reflns_used    6233
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.93
_cell_measurement_theta_min      3.20
_cell_volume                     2537.3(2)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 1997)'
_computing_data_collection       'COLLECT 2000'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12142
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.932
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.9301
_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    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.3011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6233
_reflns_number_total             8756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00311c2.cif
_cod_data_source_block           1-III
_cod_depositor_comments
'Adding full bibliography for 7220270--7220279.cif.'
_cod_database_code               7220272
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.930
_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
2. Restrained distances
 C41-O42 \\sim C41B-O42B \\sim O42-C43 \\sim O42B-C43B
 with sigma of 0.02
 C40-C41B \\sim C40-C41 \\sim C43-C44 \\sim C43B-C44
 with sigma of 0.02
3. Rigid bond restraints
 O42, O42B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43B, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O42 \\sim O42B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 
0.08
C43B \\sim C43: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 
0.08
Uanis(C41) = Uanis(C41B)
5. Others
 Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(O42B)=Sof(C43B)=
 Sof(H43C)=Sof(H43D)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(O42)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=Sof(H44A)=Sof(H44B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C28(H28), C21(H21), C14(H14), C7(H7)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C40(H40C,H40D), C41(H41A,
 H41B), C43(H43A,H43B), C41B(H41C,H41D), C43B(H43C,H43D), C44(H44A,H44B),
 C44(H44C,H44D), 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)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C23(H23), C26(H26), C16(H16), C19(H19), C9(H9), C12(H12)
6.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), C100(H10A,H10B,H10C)
;
_shelx_res_checksum              62296