#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/04/2200498.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2200498 loop_ _publ_author_name 'Dehghanpour, Saeed' 'Mahmoudkhani, Amir H.' 'Langer, Vratislav' _publ_section_title ; Redetermination of piperazine dihydrochloride monohydrate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o610 _journal_page_last o611 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C4 H12 N2 2+, 2Cl 1-, H2 O' _chemical_formula_moiety 'C4 H12 N2 2+, 2Cl 1-, H2 O' _chemical_formula_sum 'C4 H14 Cl2 N2 O' _chemical_formula_weight 177.07 _chemical_name_systematic ; Piperazine dihydrochloride monohydrate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 107.587(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.2233(3) _cell_length_b 6.3323(3) _cell_length_c 13.5389(6) _cell_measurement_reflns_used 1781 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 32 _cell_measurement_theta_min 1 _cell_volume 835.50(6) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT and SADABS (Sheldrick, 1996)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2000)' _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Bruker, 1997)' _diffrn_ambient_temperature 297(2) _diffrn_detector_area_resol_mean no _diffrn_measured_fraction_theta_full .926 _diffrn_measured_fraction_theta_max .926 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0434 _diffrn_reflns_av_sigmaI/netI .0596 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 3545 _diffrn_reflns_theta_full 32.91 _diffrn_reflns_theta_max 32.91 _diffrn_reflns_theta_min 3.16 _diffrn_standards_decay_% none _diffrn_standards_interval_count no _diffrn_standards_interval_time no _diffrn_standards_number no _exptl_absorpt_coefficient_mu .710 _exptl_absorpt_correction_T_max .9722 _exptl_absorpt_correction_T_min .7644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thin plate' _exptl_crystal_F_000 376 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .04 _refine_diff_density_max .481 _refine_diff_density_min -.347 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 51 _refine_ls_number_reflns 1453 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all .0845 _refine_ls_R_factor_gt .0518 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0792P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1489 _reflns_number_gt 974 _reflns_number_total 1453 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob6045.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 2200498 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cl1 .79885(6) .09493(10) .66349(4) .0422(2) Uani d . 1 . . Cl N1 .55069(18) .4113(3) .60246(13) .0316(4) Uani d . 1 . . N H1A .4929 .4679 .6338 .040(7) Uiso calc R 1 . . H H1B .6105 .3283 .6486 .055(8) Uiso calc R 1 . . H C1 .4714(2) .2815(3) .51244(16) .0348(5) Uani d . 1 . . C H1C .4202 .1738 .5360 .048(7) Uiso calc R 1 . . H H1D .5344 .2112 .4821 .049(8) Uiso calc R 1 . . H O1 .5000 .0430(6) .7500 .0731(9) Uani d SD 1 . . O C2 .6266(2) .5831(3) .56860(17) .0346(5) Uani d . 1 . . C H2A .6947 .5223 .5402 .029(6) Uiso calc R 1 . . H H2B .6741 .6695 .6277 .048(7) Uiso calc R 1 . . H H1 .434(4) -.035(7) .757(5) .150 Uiso d D 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 .0371(3) .0526(4) .0370(3) .0167(2) .0113(2) .0009(2) N1 .0271(8) .0362(9) .0316(8) .0039(7) .0090(6) .0020(7) C1 .0365(11) .0269(10) .0425(11) -.0020(8) .0143(9) -.0024(8) O1 .055(2) .0586(19) .112(3) .000 .035(2) .000 C2 .0259(10) .0397(11) .0372(10) -.0046(8) .0078(8) -.0061(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 . 1.487(3) yes N1 C1 . 1.491(3) yes N1 H1A . .9000 ? N1 H1B . .9000 ? C1 C2 5_666 1.510(3) yes C1 H1C . .9700 ? C1 H1D . .9700 ? O1 H1 . .86(2) ? C2 C1 5_666 1.510(3) ? C2 H2A . .9700 ? C2 H2B . .9700 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 N1 C1 . . 110.92(16) yes C2 N1 H1A . . 109.5 ? C1 N1 H1A . . 109.5 ? C2 N1 H1B . . 109.5 ? C1 N1 H1B . . 109.5 ? H1A N1 H1B . . 108.0 ? N1 C1 C2 . 5_666 111.01(17) yes N1 C1 H1C . . 109.4 ? C2 C1 H1C 5_666 . 109.4 ? N1 C1 H1D . . 109.4 ? C2 C1 H1D 5_666 . 109.4 ? H1C C1 H1D . . 108.0 ? N1 C2 C1 . 5_666 110.23(17) yes N1 C2 H2A . . 109.6 ? C1 C2 H2A 5_666 . 109.6 ? N1 C2 H2B . . 109.6 ? C1 C2 H2B 5_666 . 109.6 ? H2A C2 H2B . . 108.1 ? H1 O1 H1 . 2_656 109(7) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1B Cl1 . .90 2.39 3.1412(19) 141.4 N1 H1A Cl1 3_455 .90 2.29 3.1541(18) 162.1 O1 H1 Cl1 3_445 .86(2) 2.82(4) 3.492(3) 137(5) C2 H2B Cl1 4_656 .97 2.80 3.475(2) 127.7 _journal_paper_doi 10.1107/S1600536801009771