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_7214319
_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         'C36 H38 O8, 2(C6 H16 N), C H4 O'
_chemical_formula_sum            'C49 H74 N2 O9'
_chemical_formula_weight         835.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.0186(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6120(2)
_cell_length_b                   14.5363(2)
_cell_length_c                   27.4010(4)
_cell_measurement_reflns_used    8165
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      75.2780
_cell_measurement_theta_min      3.9070
_cell_volume                     4539.90(12)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997); MERCURY (Macrae, <i>et al.</i>, 2008)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16003
_diffrn_reflns_theta_full        69.98
_diffrn_reflns_theta_max         69.98
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_correction_T_min  0.9070
_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_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8547
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0500P)^2^+1.7158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                7434
_reflns_number_total             8547
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce42291g.txt
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7214319