#------------------------------------------------------------------------------ #$Date: 2011-10-03 12:28:05 +0300 (Mon, 03 Oct 2011) $ #$Revision: 27371 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7206441.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7206441 loop_ _publ_author_name 'Dziubek, Kamil F.' 'Katrusiak, Andrzej' _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_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) _[local]_cod_data_source_file c1cp21087d.txt _[local]_cod_data_source_block pyrrolidine_15_kbar _cod_original_cell_volume 389.96(15) _cod_database_code 7206441 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags N1 N 0.3182(7) 1.1601(16) 0.226(2) 0.030(2) Uiso 1 1 d . H1 H 0.388(8) 1.057(14) 0.239(14) 0.036 Uiso 1 1 d . C2 C 0.3360(11) 1.120(2) 0.094(3) 0.047(3) Uiso 1 1 d . H21 H 0.4613 1.1418 0.0860 0.056 Uiso 1 1 calc R H22 H 0.2846 1.2564 0.0469 0.056 Uiso 1 1 calc R C3 C 0.2399(9) 0.8283(16) 0.0365(19) 0.042(2) Uiso 1 1 d . H32 H 0.3229 0.7010 0.0342 0.051 Uiso 1 1 calc R H31 H 0.1758 0.8299 -0.0496 0.051 Uiso 1 1 calc R C4 C 0.1096(9) 0.7535(18) 0.1329(19) 0.042(2) Uiso 1 1 d . H42 H -0.0128 0.7130 0.0884 0.050 Uiso 1 1 calc R H41 H 0.1356 0.5925 0.1740 0.050 Uiso 1 1 calc R C5 C 0.1359(9) 1.0003(18) 0.232(2) 0.047(2) Uiso 1 1 d . H51 H 0.0453 1.1120 0.2112 0.056 Uiso 1 1 calc R H52 H 0.1298 0.9418 0.3168 0.056 Uiso 1 1 calc R N6 N 0.5548(8) 0.7488(13) 0.3181(14) 0.0312(17) Uiso 1 1 d . H6 H 0.470(8) 0.607(15) 0.312(14) 0.037 Uiso 1 1 d . C7 C 0.6454(9) 0.7915(19) 0.454(2) 0.042(2) Uiso 1 1 d . H71 H 0.5615 0.7328 0.5107 0.050 Uiso 1 1 calc R H72 H 0.6963 0.9850 0.4784 0.050 Uiso 1 1 calc R C8 C 0.7947(10) 0.6146(18) 0.463(2) 0.032(2) Uiso 1 1 d . H81 H 0.9106 0.7289 0.4941 0.039 Uiso 1 1 calc R H82 H 0.7732 0.4719 0.5194 0.039 Uiso 1 1 calc R C9 C 0.7860(10) 0.492(2) 0.329(2) 0.043(3) Uiso 1 1 d . H91 H 0.7218 0.3027 0.3161 0.051 Uiso 1 1 calc R H92 H 0.9044 0.4959 0.3075 0.051 Uiso 1 1 calc R C10 C 0.6842(9) 0.6808(18) 0.250(2) 0.039(2) Uiso 1 1 d . H101 H 0.7650 0.8462 0.2381 0.047 Uiso 1 1 calc R H102 H 0.6295 0.5862 0.1665 0.047 Uiso 1 1 calc R loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 N1 C5 104.0(12) n N1 C2 C3 109.7(13) n C2 C3 C4 101.7(16) n C5 C4 C3 107.0(9) n N1 C5 C4 105.4(13) n C10 N6 C7 103.8(7) n N6 C7 C8 106.4(18) n C9 C8 C7 104.7(14) n C8 C9 C10 102.3(13) n N6 C10 C9 107.2(17) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.43(3) n N1 C5 1.502(11) n C2 C3 1.537(17) n C3 C4 1.56(2) n C4 C5 1.51(2) n N6 C10 1.38(2) n N6 C7 1.48(3) n C7 C8 1.552(13) n C8 C9 1.48(3) n C9 C10 1.533(13) n