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_7229451
_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_moiety         'C18 H24 N2'
_chemical_formula_sum            'C18 H24 N2'
_chemical_formula_weight         268.39
_chemical_name_systematic
;
 4,4'-di-tert-butyl-2,2'-bipyridyl
;
_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   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-08-07 deposited with the CCDC.
2017-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.039(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3193(7)
_cell_length_b                   6.5863(3)
_cell_length_c                   10.3445(6)
_cell_measurement_reflns_used    1197
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.6447
_cell_measurement_theta_min      2.8807
_cell_volume                     820.88(8)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4348
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         28.708
_diffrn_reflns_theta_min         3.382
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       blocks
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.032(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1886
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1178
_reflns_number_total             1886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01481c2.cif
_cod_data_source_block           250
_cod_database_code               7229451
_shelxl_version_number           2013-4
_shelx_res_checksum              4891