Horning-crown diamine complexes and salts: proton transfer mediated by solid-state intermolecular hydrogen bonding
Luciawati, Fera; Higham, Luke T.; Strauss, Christopher R.; Scott, Janet L.; CrystEngComm 13 (2011) 167–; doi:10.1039/c003571h

data_7205064
_publ_section_title
;
 Horning-crown diamine complexes and salts: proton transfer mediated by
 solid-state intermolecular hydrogen bonding
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              167
_journal_paper_doi               10.1039/c003571h
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C46 H42 O6,C2 H9 N2,C2 H9 N2'
_chemical_formula_sum            'C50 H60 N4 O6'
_chemical_formula_weight         813.02
_chemical_name_common
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-
tricyclo(27.3.1.113,17) tetratriaconta-
1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol) di-
ethylenediamine salt
;
_chemical_name_systematic
;
(3,4:10,11:19,20:26,27-tetrabenzo-5,9,21,25-tetraoxa-tricyclo[27.3.1.113,17]
tetratriaconta-1(32),3,10,13,15,17(34),19,26,29(33),30-decaene-33,34-diol)
di-ethylenediamine salt
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.05(3)
_cell_angle_beta                 82.69(3)
_cell_angle_gamma                60.57(3)
_cell_formula_units_Z            2
_cell_length_a                   11.610(2)
_cell_length_b                   11.669(2)
_cell_length_c                   18.732(4)
_cell_measurement_temperature    123(2)
_cell_volume                     2161.4(10)
_computing_cell_refinement       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_molecular_graphics    X-seed
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35285
_diffrn_reflns_theta_full        29.05
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         11323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+2.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1704
_reflns_number_gt                10149
_reflns_number_total             11323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C003571H.TXT
_cod_data_source_block           2d
_cod_depositor_comments
;
The following automatic conversions were performed:
'__exptl_crystal_density_diffrn' tag replaced with
'_exptl_crystal_density_diffrn'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2161.5(7)
_cod_database_code               7205064