Deprotonation of resorcinarenes by mono- and diamine bases: complexation and intermolecular interactions in the solid state
Beyeh, N. Kodiah; Valkonen, Arto; Rissanen, Kari; CrystEngComm 16 (2014) 3758–; doi:10.1039/c3ce42291g

data_7214321
_publ_section_title
;
 Deprotonation of resorcinarenes by mono- and diamine bases: complexation
 and intermolecular interactions in the solid state
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3758
_journal_paper_doi               10.1039/c3ce42291g
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C40 H47 O8, C3 H8 N, C H4 O, 2(C3 H7 N)'
_chemical_formula_sum            'C50 H73 N3 O9'
_chemical_formula_weight         860.11
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                107.092(2)
_cell_angle_beta                 94.407(2)
_cell_angle_gamma                110.946(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7076(5)
_cell_length_b                   14.7176(6)
_cell_length_c                   15.4943(6)
_cell_measurement_temperature    173(2)
_cell_volume                     2333.23(17)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker, 2008)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997); MERCURY (Macrae, <i>et al.</i>, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR-2011 (Burla <i>et al.</i>, 2012)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius Kappa CCD with APEXII detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29369
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.291
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0965 before and 0.0848 after correction.
The Ratio of minimum to maximum transmission is 0.7841.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8194
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0456P)^2^+3.2979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5833
_reflns_number_total             8194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce42291g.txt
_cod_data_source_block           III
_cod_database_code               7214321
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.990