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_7225676
_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 H Cl2 O4, C7 H10 N   
;
_chemical_formula_sum            'C13 H11 Cl2 N O4'
_chemical_formula_weight         316.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_update_record
;
2016-05-04 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7415(2)
_cell_length_b                   11.0538(3)
_cell_length_c                   15.4495(3)
_cell_measurement_reflns_used    14007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.62
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     1315.94(6)
_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 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.1033147
_diffrn_orient_matrix_UB_12      0.255648E-1
_diffrn_orient_matrix_UB_13      0.296625E-1
_diffrn_orient_matrix_UB_21      -0.682196E-1
_diffrn_orient_matrix_UB_22      0.104143E-1
_diffrn_orient_matrix_UB_23      -0.578402E-1
_diffrn_orient_matrix_UB_31      -0.389042E-1
_diffrn_orient_matrix_UB_32      -0.861522E-1
_diffrn_orient_matrix_UB_33      0.018102E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74589
_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        50.62
_diffrn_reflns_theta_max         50.62
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.5344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.064(13)
_refine_ls_extinction_expression
;
        Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         11797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.00001
_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         0.021
_reflns_number_gt                11375
_reflns_number_total             14007
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ce01065b3.cif
_cod_data_source_block           1_(2,5)_xd
_cod_depositor_comments
'Adding full bibliography for 7225667--7225698.cif.'
_cod_database_code               7225676