#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202331.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_2202331 loop_ _publ_author_name 'Srinivasan, Bikshandarkoil R. ' 'N\"ather, Christian' 'Bensch, Wolfgang' _publ_section_title ; Piperazinium chromate(VI) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m639 _journal_page_last m641 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C4 H12 N2 2+, O4 Cr 2-' _chemical_formula_moiety 'C4 H12 N2 2+, O4 Cr 2-' _chemical_formula_sum 'C4 H12 Cr N2 O4' _chemical_formula_weight 204.16 _chemical_name_common 'Piperazinium chromate(VI)' _chemical_name_systematic ; Piperazinium chromate(VI) ; _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 93.766(12) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.6651(9) _cell_length_b 12.3726(18) _cell_length_c 8.4886(10) _cell_measurement_reflns_used 105 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 16 _cell_volume 803.30(18) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1992)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1992)' _computing_molecular_graphics 'XP in SHELXTL (Bruker, 1998)' _computing_publication_material 'CIFTAB in SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe AED-II four-circle' _diffrn_measurement_method \w _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 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4578 _diffrn_reflns_theta_full 30.03 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_min 2.91 _diffrn_standards_decay_% none _diffrn_standards_interval_time 120 _diffrn_standards_number 4 _exptl_absorpt_coefficient_mu 1.396 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE and X-RED; Stoe & Cie, 1998)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 424 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.363 _refine_diff_density_min -0.523 _refine_ls_extinction_coef 0.105(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 2350 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0263 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.3211P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.0818 _reflns_number_gt 2034 _reflns_number_total 2350 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bt6299.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2202331 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Cr1 0.21819(3) 0.910006(19) 0.17835(3) 0.02268(10) Uani d . 1 . . Cr O1 0.03085(15) 0.90257(10) 0.26610(15) 0.0314(2) Uani d . 1 . . O O2 0.20805(17) 0.81921(11) 0.03380(13) 0.0346(3) Uani d . 1 . . O O3 0.38107(15) 0.88111(13) 0.30737(14) 0.0392(3) Uani d . 1 . . O O4 0.2389(2) 1.02997(12) 0.10613(18) 0.0495(4) Uani d . 1 . . O N1 0.14987(18) 0.91284(11) 0.74774(15) 0.0270(3) Uani d . 1 . . N H1N1 0.0788 0.9706 0.7508 0.032 Uiso calc R 1 . . H H2N1 0.1610 0.8842 0.8453 0.032 Uiso calc R 1 . . H C1 0.0691(2) 0.83133(14) 0.63617(18) 0.0291(3) Uani d . 1 . . C H1A 0.0490 0.8631 0.5321 0.035 Uiso calc R 1 . . H H1B -0.0426 0.8083 0.6719 0.035 Uiso calc R 1 . . H C2 0.1892(2) 0.73577(14) 0.6280(2) 0.0328(3) Uani d . 1 . . C H2A 0.2012 0.7006 0.7303 0.039 Uiso calc R 1 . . H H2B 0.1395 0.6841 0.5518 0.039 Uiso calc R 1 . . H N2 0.36406(18) 0.77052(13) 0.58131(16) 0.0330(3) Uani d . 1 . . N H1N2 0.3535 0.7987 0.4834 0.040 Uiso calc R 1 . . H H2N2 0.4349 0.7126 0.5793 0.040 Uiso calc R 1 . . H C3 0.4435(2) 0.85223(15) 0.6925(2) 0.0343(3) Uani d . 1 . . C H3A 0.5551 0.8755 0.6569 0.041 Uiso calc R 1 . . H H3B 0.4638 0.8204 0.7966 0.041 Uiso calc R 1 . . H C4 0.3232(2) 0.94819(14) 0.7014(2) 0.0334(3) Uani d . 1 . . C H4A 0.3729 0.9997 0.7780 0.040 Uiso calc R 1 . . H H4B 0.3110 0.9837 0.5994 0.040 Uiso calc R 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 Cr1 0.02214(14) 0.02577(14) 0.01977(13) -0.00299(8) -0.00120(8) 0.00162(8) O1 0.0264(5) 0.0316(6) 0.0369(6) 0.0027(4) 0.0064(4) -0.0005(5) O2 0.0438(7) 0.0370(7) 0.0232(5) -0.0006(5) 0.0033(5) -0.0036(4) O3 0.0258(5) 0.0605(9) 0.0304(6) -0.0027(5) -0.0055(4) 0.0051(6) O4 0.0655(9) 0.0360(7) 0.0462(7) -0.0165(7) -0.0024(7) 0.0122(6) N1 0.0289(6) 0.0278(6) 0.0245(6) 0.0051(5) 0.0034(5) -0.0006(5) C1 0.0250(6) 0.0326(8) 0.0294(7) -0.0016(6) -0.0019(5) 0.0018(6) C2 0.0413(8) 0.0237(7) 0.0324(7) -0.0016(6) -0.0048(6) -0.0023(6) N2 0.0330(6) 0.0370(7) 0.0285(6) 0.0144(6) -0.0009(5) -0.0042(6) C3 0.0233(7) 0.0395(9) 0.0395(8) 0.0018(6) -0.0017(6) -0.0024(7) C4 0.0314(7) 0.0257(7) 0.0432(9) -0.0036(6) 0.0031(6) -0.0020(7) 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 Cr1 O4 . 1.6176(14) y Cr1 O3 . 1.6451(12) y Cr1 O2 . 1.6617(12) y Cr1 O1 . 1.6631(12) y N1 C4 . 1.476(2) y N1 C1 . 1.490(2) y N1 H1N1 . 0.9000 n N1 H2N1 . 0.9000 n C1 C2 . 1.503(2) y C1 H1A . 0.9700 n C1 H1B . 0.9700 n C2 N2 . 1.486(2) y C2 H2A . 0.9700 n C2 H2B . 0.9700 n N2 C3 . 1.486(2) y N2 H1N2 . 0.9000 n N2 H2N2 . 0.9000 n C3 C4 . 1.508(2) y C3 H3A . 0.9700 n C3 H3B . 0.9700 n C4 H4A . 0.9700 n C4 H4B . 0.9700 n 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 O4 Cr1 O3 111.27(8) y O4 Cr1 O2 109.97(7) y O3 Cr1 O2 109.96(7) y O4 Cr1 O1 109.23(8) y O3 Cr1 O1 109.25(6) y O2 Cr1 O1 107.07(6) y C4 N1 C1 112.01(12) y C4 N1 H1N1 109.2 n C1 N1 H1N1 109.2 n C4 N1 H2N1 109.2 n C1 N1 H2N1 109.2 n H1N1 N1 H2N1 107.9 n N1 C1 C2 109.36(13) y N1 C1 H1A 109.8 n C2 C1 H1A 109.8 n N1 C1 H1B 109.8 n C2 C1 H1B 109.8 n H1A C1 H1B 108.3 n N2 C2 C1 110.52(14) y N2 C2 H2A 109.5 n C1 C2 H2A 109.5 n N2 C2 H2B 109.5 n C1 C2 H2B 109.5 n H2A C2 H2B 108.1 n C2 N2 C3 111.48(12) y C2 N2 H1N2 109.3 n C3 N2 H1N2 109.3 n C2 N2 H2N2 109.3 n C3 N2 H2N2 109.3 n H1N2 N2 H2N2 108.0 n N2 C3 C4 109.94(13) y N2 C3 H3A 109.7 n C4 C3 H3A 109.7 n N2 C3 H3B 109.7 n C4 C3 H3B 109.7 n H3A C3 H3B 108.2 n N1 C4 C3 110.10(14) y N1 C4 H4A 109.6 n C3 C4 H4A 109.6 n N1 C4 H4B 109.6 n C3 C4 H4B 109.6 n H4A C4 H4B 108.2 n 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 H1N1 O1 3_576 0.90 1.78 2.6697(18) 169 N1 H2N1 O2 1_556 0.90 1.81 2.7009(18) 173 N2 H1N2 O3 . 0.90 1.83 2.709(2) 164 N2 H2N2 O2 4_676 0.90 2.19 2.9133(19) 137 N2 H2N2 O1 4_676 0.90 2.22 2.9014(19) 132 _cod_database_fobs_code 2202331 _journal_paper_doi 10.1107/S1600536803014879