Structures and phase transitions in the neat 4,4'-di-tert-butyl-2,2'-bipyridyl and in its molecular complexes with either brom- or iodanilic acid
Rok, Magdalena; Szklarz, Przemyslaw; Moskwa, Marcin; Kijewska, Monika; Baran, Jan; Bator, Grazyna; Medycki, Wojciech; Zamponi, Michaela; CrystEngComm  (2017) –; doi:10.1039/C7CE01481C

data_7229448
_publ_section_title
;
 Structures and phase transitions in the neat
 4,4'-di-tert-butyl-2,2'-bipyridyl and in its molecular complexes with
 either brom- or iodanilic acid
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01481C
_journal_year                    2017
_chemical_formula_sum            'C24 H26 Br2 N2 O4'
_chemical_formula_weight         566.29
_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
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-10-02 deposited with the CCDC.
2017-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                98.84(3)
_cell_angle_beta                 104.58(6)
_cell_angle_gamma                93.42(4)
_cell_formula_units_Z            2
_cell_length_a                   8.951(3)
_cell_length_b                   11.491(5)
_cell_length_c                   11.910(3)
_cell_measurement_reflns_used    7802
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.7423
_cell_measurement_theta_min      3.0867
_cell_volume                     1165.3(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.745
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.745
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17495
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         36.830
_diffrn_reflns_theta_min         3.093
_exptl_absorpt_coefficient_mu    3.512
_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       blocks
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.3952
_exptl_crystal_size_mid          0.2236
_exptl_crystal_size_min          0.1567
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.720
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         8710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0985P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4801
_reflns_number_total             8710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01481c2.cif
_cod_data_source_block           dtbbpbra
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '__diffrn_radiation_source' replaced with
'_diffrn_radiation_source'.

Automatic conversion script
Id: cif_correct_tags 4968 2017-02-21 14:55:21Z antanas 
;
_cod_database_code               7229448
_shelxl_version_number           2013-4
_shelx_res_checksum              72306