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_7225679
_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_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                 100.451(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0870(3)
_cell_length_b                   11.4214(5)
_cell_length_c                   10.3253(4)
_cell_measurement_reflns_used    10037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.64
_cell_measurement_theta_min      1
_cell_measurement_wavelength     0.71073
_cell_volume                     937.87(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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      -0.1016472
_diffrn_orient_matrix_UB_12      -0.514523E-1
_diffrn_orient_matrix_UB_13      -0.118218E-1
_diffrn_orient_matrix_UB_21      0.362709E-1
_diffrn_orient_matrix_UB_22      -0.381233E-1
_diffrn_orient_matrix_UB_23      -0.775134E-1
_diffrn_orient_matrix_UB_31      0.644694E-1
_diffrn_orient_matrix_UB_32      -0.596751E-1
_diffrn_orient_matrix_UB_33      0.597121E-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  0.0278
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10037
_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        50.64
_diffrn_reflns_theta_max         50.64
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.7494
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.029
_refine_ls_extinction_coef       0.028(15)
_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   1.171
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         8919
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.023
_refine_ls_R_factor_gt           0.015
_refine_ls_shift/su_max          0.00006
_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         0.019
_reflns_number_gt                8718
_reflns_number_total             10037
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6ce01065b3.cif
_cod_data_source_block           2_(2,5)_xd
_cod_depositor_comments
'Adding full bibliography for 7225667--7225698.cif.'
_cod_database_code               7225679