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_7225671
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_update_record
;
2016-05-04 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                96.274(2)
_cell_angle_beta                 91.960(2)
_cell_angle_gamma                90.6090(10)
_cell_formula_units_Z            2
_cell_length_a                   5.0687(2)
_cell_length_b                   11.2561(4)
_cell_length_c                   11.6281(3)
_cell_measurement_reflns_used    13978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.44
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     659.00(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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      0.344261E-1
_diffrn_orient_matrix_UB_12      -0.777945E-1
_diffrn_orient_matrix_UB_13      -0.468051E-1
_diffrn_orient_matrix_UB_21      -0.1902439
_diffrn_orient_matrix_UB_22      -0.233391E-1
_diffrn_orient_matrix_UB_23      0.36180E-2
_diffrn_orient_matrix_UB_31      -0.400009E-1
_diffrn_orient_matrix_UB_32      0.372261E-1
_diffrn_orient_matrix_UB_33      -0.727386E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13978
_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        50.66
_diffrn_reflns_theta_max         50.66
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.7495
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.028(8)
_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   1.204
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         12502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.022
_refine_ls_R_factor_gt           0.016
_refine_ls_shift/su_max          0.00005
_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         0.02
_reflns_number_gt                12202
_reflns_number_total             13978
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ce01065b3.cif
_cod_data_source_block           1_(2,4)_xd
_cod_depositor_comments
'Adding full bibliography for 7225667--7225698.cif.'
_cod_database_code               7225671