Systematic experimental charge density analysis of anion receptor complexes.
Kirby, Isabelle L.; Brightwell, Mark; Pitak, Mateusz B.; Wilson, Claire; Coles, Simon J.; Gale, Philip A.; Physical chemistry chemical physics : PCCP 16 (2014) 10943–10958; doi:10.1039/c3cp54858a

data_7215467
_publ_section_title
;
 Systematic experimental charge density analysis of anion receptor
 complexes.
;
_journal_issue                   22
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              10943
_journal_page_last               10958
_journal_paper_doi               10.1039/c3cp54858a
_journal_volume                  16
_journal_year                    2014
_chemical_compound_source        'Isabelle Kirby'
_chemical_formula_moiety         'C13 H10 N4 O5, C4 H12 N, Cl'
_chemical_formula_sum            'C17 H22 Cl N5 O5'
_chemical_formula_weight         411.85
_chemical_name_systematic
;
 1,3-bis(4-nitrophenyl)urea with tetramethylammonium chloride
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                83.1860(10)
_cell_angle_beta                 71.662(2)
_cell_angle_gamma                80.423(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6033(2)
_cell_length_b                   11.4827(3)
_cell_length_c                   11.8705(4)
_cell_measurement_reflns_used    21504
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     967.59(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25085
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        54.02
_diffrn_reflns_theta_max         55.40
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.8708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         17926
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.029
_reflns_number_gt                18067
_reflns_number_total             25085
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3cp54858a2.cif
_cod_data_source_block           crystalstructure_4
_cod_depositor_comments
'Adding full bibliography for 7215467--7215471.cif.'
_cod_database_code               7215467