Density, freezing and molecular aggregation in pyridazine, pyridine and benzene
Podsiadło, Marcin; Jakóbek, Katarzyna; Katrusiak, Andrzej; CrystEngComm 12 (2010) 2561–; doi:10.1039/c001153c

data_7212505
_publ_section_title
;
 Density, freezing and molecular aggregation in pyridazine, pyridine and
 benzene
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              2561
_journal_paper_doi               10.1039/c001153c
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C4 H4 N2'
_chemical_formula_sum            'C4 H4 N2'
_chemical_formula_weight         80.09
_chemical_melting_point          265
_chemical_name_common            pyridazine
_chemical_name_systematic
;
pyridazine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.8432(8)
_cell_length_b                   10.964(2)
_cell_length_c                   9.778(2)
_cell_measurement_reflns_used    2829
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      4.17
_cell_volume                     411.93(14)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2004)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2004)'
_computing_data_reduction
'CrysAlisRED (Oxford Diffraction, 2004); REDSHABS (Katrusiak, A. 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL--97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS--97 (Sheldrick, 1997)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         270000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.414
_diffrn_measured_fraction_theta_max 0.414
_diffrn_measurement_device_type  'KM-4 CCD'
_diffrn_measurement_method       '\f- and \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  0.1052
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2829
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         4.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Correction for absorption of the diamond-anvil cell and the sample
were made using program REDSHABS (Katrusiak, A. (2003) REDSHABS. Adam
Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.109
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.026
_refine_ls_extinction_coef       0.81(13)
_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   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         301
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+0.1292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                234
_reflns_number_total             301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001153c.txt
_cod_data_source_block           1pir_0.27GPa
_cod_original_cell_volume        411.95(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7212505