Pressure-induced pseudorotation in crystalline pyrrolidine.
Dziubek, Kamil F.; Katrusiak, Andrzej; Physical chemistry chemical physics : PCCP 13 (2011) 15428–15431; doi:10.1039/c1cp21087d

data_7206441
_publ_section_title
;
 Pressure-induced pseudorotation in crystalline pyrrolidine.
;
_journal_issue                   34
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              15428
_journal_page_last               15431
_journal_paper_doi               10.1039/c1cp21087d
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C4 H9 N'
_chemical_formula_sum            'C4 H9 N'
_chemical_formula_weight         71.12
_chemical_melting_point          210.15
_chemical_name_common            pyrrolidine
_chemical_name_systematic
;
azacyclopentane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.37(3)
_cell_angle_beta                 98.54(3)
_cell_angle_gamma                99.59(3)
_cell_formula_units_Z            4
_cell_length_a                   7.702(2)
_cell_length_b                   4.9380(10)
_cell_length_c                   10.572(2)
_cell_measurement_reflns_used    666
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.78
_cell_volume                     389.96(16)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_reduction
'CrysAlisPro (Oxford Diffraction, 2010); REDSHADE (Katrusiak, A. 2003)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_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         1500000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.321
_diffrn_measured_fraction_theta_max 0.321
_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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2002
_diffrn_reflns_theta_full        24.88
_diffrn_reflns_theta_max         24.88
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Corrections for absorption of the diamond-anvil cell and the sample
were made using program REDSHADE [Katrusiak, A. (2003) REDSHADE. Adam
Mickiewicz University Pozna\'n; Katrusiak, A. (2004) Z. Kristallogr.
219, 461-467].
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             160
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.17
_refine_diff_density_max         0.123
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0764
_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^)+(0.0903P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                259
_reflns_number_total             434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cp21087d.txt
_cod_data_source_block           pyrrolidine_15_kbar
_cod_original_cell_volume        389.96(15)
_cod_database_code               7206441