Comparison of computationally cheap methods for providing insight into the crystal packing of highly bromomethylated azobenzenes
Vande Velde, Christophe M. L.; Zeller, Matthias; Azov, Vladimir A.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618015309

data_2021362
_publ_section_title
;
 Comparison of computationally cheap methods for providing insight into
 the crystal packing of highly bromomethylated azobenzenes
;
_journal_coeditor_code           KY3150
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618015309
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C14 H11 Br3 N2'
_chemical_formula_moiety         'C14 H11 Br3 N2'
_chemical_formula_sum            'C14 H11 Br3 N2'
_chemical_formula_weight         446.98
_chemical_melting_point          420.1(10)
_chemical_name_systematic
;
(<i>E</i>)-[4-(Bromomethyl)phenyl][4-(dibromomethyl)phenyl]diazene
;
_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_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 99.692(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5380(10)
_cell_length_b                   5.2830(10)
_cell_length_c                   32.801(4)
_cell_measurement_reflns_used    6003
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.98
_cell_measurement_theta_min      2.52
_cell_volume                     1458.4(4)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015) and
<i>shelXle</i>(H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            13694
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.365
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    8.285
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.3155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+4.4145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                3947
_reflns_number_total             4445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3150sup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '146--148 C' was changed to
'420.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               2021362
_cod_database_fobs_code          2021362
_shelx_estimated_absorpt_t_min   0.118
_shelx_estimated_absorpt_t_max   0.317
_shelx_hkl_checksum              46361
_shelx_res_checksum              69090