Anisotropic displacement parameters from dispersion-corrected DFT methods and their experimental validation by temperature-dependent X-ray diffraction
George, Janine; Wang, Ai; Deringer, Volker L.; Wang, Ruimin; Dronskowski, Richard; Englert, Ulli; CrystEngComm 17 (2015) 7414–; doi:10.1039/C5CE01219H

data_7221874
_publ_section_title
;
 Anisotropic displacement parameters from dispersion-corrected DFT methods
 and their experimental validation by temperature-dependent X-ray
 diffraction
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              7414
_journal_paper_doi               10.1039/C5CE01219H
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C5 Cl5 N'
_chemical_formula_sum            'C5 Cl5 N'
_chemical_formula_weight         251.31
_chemical_name_common            C5CL5N_250K
_chemical_name_systematic        Pentachloropyridine
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-21 deposited with the CCDC.
2015-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.003(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.3426(15)
_cell_length_b                   5.2051(15)
_cell_length_c                   15.021(4)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.77
_cell_volume                     411.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2999
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.760
_diffrn_reflns_theta_min         2.754
_diffrn_source                   'Incoatec microsource'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_description       plate
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 370 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0336P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_full    0.746
_reflns_Friedel_fraction_max     0.593
_reflns_number_gt                1361
_reflns_number_total             1939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01219h2.cif
_cod_data_source_block           C5CL5N_250K
_cod_depositor_comments
'Adding full bibliography for 7221871--7221875.cif.'
_cod_database_code               7221874
_shelx_estimated_absorpt_t_min   0.6077
_shelx_estimated_absorpt_t_max   0.7461
_shelxl_version_number           2013-2
_shelx_res_checksum              87495