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_7229449
_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   mixed
_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                80.595(6)
_cell_angle_beta                 66.706(6)
_cell_angle_gamma                79.529(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8323(5)
_cell_length_b                   11.7934(6)
_cell_length_c                   12.0531(11)
_cell_measurement_reflns_used    2206
_cell_measurement_temperature    345(2)
_cell_measurement_theta_max      29.6390
_cell_measurement_theta_min      3.7110
_cell_volume                     1255.83(16)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      345(2)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.807
_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  0.0169
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10416
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.865
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.536
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78930
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.3731
_exptl_crystal_size_mid          0.3117
_exptl_crystal_size_min          0.1586
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.0087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4005
_reflns_number_total             6397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01481c2.cif
_cod_data_source_block           moskw2
_cod_database_code               7229449
_shelxl_version_number           2013-4
_shelx_res_checksum              84743