Macrocyclic bis(ureas) as ligands for anion complexation.
Kretschmer, Claudia; Dittmann, Gertrud; Beck, Johannes; Beilstein journal of organic chemistry 10 (2014) 1834–1839; doi:10.3762/bjoc.10.193

data_4029846
_publ_section_title
;
 Macrocyclic bis(ureas) as ligands for anion complexation.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              1834
_journal_page_last               1839
_journal_paper_doi               10.3762/bjoc.10.193
_journal_volume                  10
_journal_year                    2014
_chemical_formula_moiety         'C42 H36 Br1 N5 O2'
_chemical_formula_sum            'C42 H40 Br N5 O2'
_chemical_formula_weight         726.70
_chemical_name_systematic
;
Tetraethylammonium-cyclo-bis(butadiynyldiphenylurea)-bromide complex 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.548(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7152(6)
_cell_length_b                   17.5556(8)
_cell_length_c                   20.5472(8)
_cell_measurement_reflns_used    7920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.91
_cell_volume                     3731.8(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'HKL Denzo and Scalepack (Otwinowski & Minor'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.1425
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32096
_diffrn_reflns_theta_full        25.40
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.9225
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Department of Chemistry
University of Anywhere
Sometown
Somewhere, UK
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0573P)^2^+1.5843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                3078
_reflns_number_total             6837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-10-193-S2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4029844--4029847.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4029846