High resolution X-ray and neutron diffraction studies on molecular complexes of chloranilic acid and lutidines
Sovago, Ioana; Thomas, Lynne H.; Adam, Martin S.; Capelli, Silvia C.; Wilson, Chick C.; Farrugia, Louis J.; CrystEngComm 18 (2016) 5697–; doi:10.1039/C6CE01065B

data_7225685
_publ_section_title
;
 High resolution X-ray and neutron diffraction studies on molecular
 complexes of chloranilic acid and lutidines
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5697
_journal_paper_doi               10.1039/C6CE01065B
_journal_volume                  18
_journal_year                    2016
_chemical_compound_source        commercial
_chemical_formula_moiety
;
C6 Cl2 O4, 2(C7 H10 N)  
;
_chemical_formula_sum            'C20 H20 Cl2 N2 O4'
_chemical_formula_weight         423.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_update_record
;
2016-05-04 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.526(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1427(3)
_cell_length_b                   9.3025(4)
_cell_length_c                   14.7753(6)
_cell_measurement_reflns_used    5216
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.9
_cell_measurement_theta_min      3.5
_cell_measurement_wavelength     0.9484
_cell_volume                     978.68(7)
_computing_cell_refinement       'Dirax (Duisenberg, 1992)'
_computing_data_collection       'ILL-MAD software'
_computing_data_reduction        'PFIND, RETREAT (Wilkinson et al.,1988)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'multiwire proportional chamber'
_diffrn_detector_area_resol_mean 0.52
_diffrn_detector_details
;
ILL cylindrically shaped large-area position sensitive detector 
with 120 by 30 deg detection angle (resolution: 0.4 by 0.64 pixels/mm)
;
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.79
_diffrn_measurement_device_type  '4-circles Eulerian cradle'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Cu(220)
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'nuclear reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.9484
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.79
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5216
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.79
_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        34.683
_diffrn_reflns_theta_max         61.891
_diffrn_reflns_theta_min         3.457
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.1665
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             238
_exptl_crystal_size_max          4
_exptl_crystal_size_mid          3
_exptl_crystal_size_min          2
_refine_diff_density_max         4.145
_refine_diff_density_min         -2.234
_refine_diff_density_rms         0.402
_refine_ls_extinction_coef       0.0035(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.223
_refine_ls_wR_factor_ref         0.2545
_reflns_Friedel_coverage         0
_reflns_number_gt                3316
_reflns_number_total             5216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01065b3.cif
_cod_data_source_block           2_(2,6)_neutron
_cod_depositor_comments
'Adding full bibliography for 7225667--7225698.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7225685