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_7229450
_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 I2 N2 O4'
_chemical_formula_weight         660.27
_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                99.09(4)
_cell_angle_beta                 103.48(5)
_cell_angle_gamma                94.58(4)
_cell_formula_units_Z            2
_cell_length_a                   9.261(3)
_cell_length_b                   11.779(3)
_cell_length_c                   11.997(4)
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.0973
_cell_measurement_theta_min      2.7016
_cell_volume                     1247.3(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9785
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         30.164
_diffrn_reflns_theta_min         2.707
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.2835
_exptl_crystal_size_mid          0.1635
_exptl_crystal_size_min          0.1221
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.1498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4927
_reflns_number_total             6360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01481c2.cif
_cod_data_source_block           dtbbpialt
_cod_database_code               7229450
_shelxl_version_number           2013-4
_shelx_res_checksum              91043