#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/17/2011738.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_2011738 loop_ _publ_author_name 'Melnyk, Oksana P.' 'Schollmeyer, Dieter' 'Olijnyk, Volodymyr V.' 'Filinchuk, Yaroslav E.' _publ_section_title ; (\h^2^-Allylammonium)aquabis(sulfamato-N)copper(I) ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 151 _journal_page_last 153 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu (C3 H8 N) (NH2 S O3)2 (H2 O)]' _chemical_formula_moiety 'C3 H14 Cu N3 O7 S2' _chemical_formula_sum 'C3 H14 Cu N3 O7 S2' _chemical_formula_weight 331.83 _chemical_name_systematic ; aqua(\h^2^-allylammonium)bis(sulfamato-N)copper(I) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90.00 _cell_angle_beta 103.593(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.5437(5) _cell_length_b 8.89230(10) _cell_length_c 9.7121(4) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 37 _cell_measurement_theta_min 32.5 _cell_volume 1136.91(6) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf Nonius, 1994)' _computing_data_reduction 'Corinc (Dr\"ager & Gattow, 1971)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full .937 _diffrn_measured_fraction_theta_max .937 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'rotating anode' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0154 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2332 _diffrn_reflns_theta_full 74.65 _diffrn_reflns_theta_max 74.65 _diffrn_reflns_theta_min 3.36 _diffrn_standards_decay_% 'no decay, variation 0.5' _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.451 _exptl_absorpt_correction_T_max .739 _exptl_absorpt_correction_T_min .359 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_process_details '(Corinc; Dr\"ager & Gattow, 1971)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_meas 1.92 _exptl_crystal_density_method 'flotation in CHCl~3~/CHBr~3~ mixture' _exptl_crystal_description plate _exptl_crystal_F_000 680 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .05 _refine_diff_density_max .738 _refine_diff_density_min -.776 _refine_ls_extinction_coef .0070(5) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 170 _refine_ls_number_reflns 2332 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.251 _refine_ls_R_factor_all .0420 _refine_ls_R_factor_gt .0417 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0575P)^2^+2.2982P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1167 _reflns_number_gt 2303 _reflns_number_total 2332 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file av1052.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2011738 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Cu .21481(3) .44817(5) .33716(5) .0174(2) Uani d . 1 . . Cu S1 .02568(5) .28010(8) .41619(8) .0173(2) Uani d . 1 . . S S2 .36509(5) .17255(8) .39079(7) .0167(2) Uani d . 1 . . S O1 .0771(2) .1461(3) .3855(3) .0280(5) Uani d . 1 . . O O2 .0582(3) .3308(4) .5598(3) .0445(8) Uani d . 1 . . O O3 -.0830(2) .2706(3) .3647(4) .0443(8) Uani d . 1 . . O O4 .3746(2) .0161(3) .3606(4) .0426(7) Uani d . 1 . . O O5 .44758(17) .2618(3) .3620(2) .0232(5) Uani d . 1 . . O O6 .3459(2) .2022(3) .5285(3) .0331(6) Uani d . 1 . . O O7 .1960(2) .5313(3) .1029(3) .0244(5) Uani d . 1 . . O H13 .173(4) .483(6) .043(6) .036(14) Uiso d . 1 . . H H14 .167(4) .594(6) .100(5) .029(13) Uiso d . 1 . . H N1 .0622(2) .4155(3) .3166(3) .0226(6) Uani d . 1 . . N H1 .0353 .5031 .3365 .043(13) Uiso calc R 1 . . H H2 .0343 .3945 .2251 .08(2) Uiso calc R 1 . . H N2 .26068(19) .2417(3) .2771(3) .0156(5) Uani d . 1 . . N H3 .2094 .1756 .2703 .028(11) Uiso calc R 1 . . H H4 .2737 .2505 .1908 .038(12) Uiso calc R 1 . . H N3 .4089(2) .5527(3) .2168(3) .0244(6) Uani d G 1 . . N H10 .4356 .4730 .2583 .052(16) Uiso calc G 1 . . H H11 .4518 .5975 .1795 .031(11) Uiso calc G 1 . . H H12 .3566 .5296 .1524 .042(14) Uiso calc G 1 . . H C1 .2527(3) .6328(5) .4624(5) .0375(9) Uani d . 1 . . C H5 .2225 .7201 .4191 .034(12) Uiso calc R 1 . . H H6 .2240 .5824 .5274 .066(18) Uiso calc R 1 . . H C2 .3385(3) .5788(4) .4305(4) .0238(7) Uani d . 1 . . C H7 .3679 .4914 .4745 .058(16) Uiso calc R 1 . . H C3 .3873(3) .6568(4) .3260(4) .0265(7) Uani d . 1 . . C H8 .3427 .7364 .2795 .055(15) Uiso calc R 1 . . H H9 .4504 .7029 .3766 .048(14) 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 Cu .0166(3) .0126(3) .0257(3) -.00059(16) .01033(19) -.00149(16) S1 .0193(4) .0148(4) .0204(4) -.0009(3) .0102(3) .0031(3) S2 .0201(4) .0126(4) .0194(4) .0056(3) .0087(3) .0033(3) O1 .0390(14) .0158(11) .0313(12) .0042(10) .0123(11) .0031(9) O2 .071(2) .0427(17) .0188(12) .0113(15) .0085(13) -.0027(11) O3 .0201(13) .0383(16) .075(2) -.0061(11) .0128(13) .0182(15) O4 .0473(17) .0126(12) .066(2) .0114(11) .0096(15) -.0014(12) O5 .0185(11) .0274(12) .0254(11) .0019(9) .0081(9) .0040(9) O6 .0414(15) .0455(16) .0166(11) .0064(12) .0152(10) .0092(11) O7 .0262(13) .0169(12) .0289(14) .0043(11) .0040(10) -.0023(10) N1 .0162(12) .0184(13) .0352(15) .0028(10) .0104(11) .0115(11) N2 .0155(12) .0138(11) .0185(12) .0013(9) .0060(9) -.0004(9) N3 .0244(14) .0228(15) .0305(15) -.0097(11) .0154(12) -.0040(12) C1 .048(2) .0277(19) .043(2) -.0078(17) .0238(19) -.0206(17) C2 .0305(17) .0189(15) .0231(15) -.0068(13) .0083(13) -.0084(13) C3 .0330(18) .0165(15) .0321(17) -.0123(13) .0119(14) -.0072(13) 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 Cu C1 . 2.035(4) yes Cu N1 . 2.050(3) yes Cu C2 . 2.066(3) yes Cu N2 . 2.066(3) yes Cu O7 . 2.348(3) yes S1 O2 . 1.433(3) ? S1 O3 . 1.442(3) ? S1 O1 . 1.447(3) ? S1 N1 . 1.690(3) yes S2 O4 . 1.433(3) ? S2 O6 . 1.446(2) ? S2 O5 . 1.450(2) ? S2 N2 . 1.692(3) yes N3 C3 . 1.488(4) ? C1 C2 . 1.359(5) yes C2 C3 . 1.504(5) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 '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 .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0492 .0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .3331 .5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 .5888 '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 C1 Cu N1 106.21(15) ? C1 Cu C2 38.70(15) yes N1 Cu C2 144.88(13) ? C1 Cu N2 146.63(15) ? N1 Cu N2 102.11(11) yes C2 Cu N2 110.92(12) ? C1 Cu O7 106.23(15) ? N1 Cu O7 94.19(11) yes C2 Cu O7 98.05(12) ? N2 Cu O7 88.73(10) yes O2 S1 O3 114.3(2) ? O2 S1 O1 114.02(17) ? O3 S1 O1 112.47(18) ? O2 S1 N1 105.59(18) ? O3 S1 N1 104.81(16) ? O1 S1 N1 104.42(14) ? O4 S2 O6 114.23(19) ? O4 S2 O5 112.45(17) ? O6 S2 O5 113.12(16) ? O4 S2 N2 108.69(16) ? O6 S2 N2 103.45(14) ? O5 S2 N2 103.82(13) ? S1 N1 Cu 117.98(15) yes S2 N2 Cu 113.55(13) yes C2 C1 Cu 71.8(2) ? C1 C2 C3 121.7(4) ? C1 C2 Cu 69.5(2) ? C3 C2 Cu 113.7(2) ? N3 C3 C2 112.6(3) ? 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 _geom_hbond_publ_flag O7 H13 O1 4_565 .73(6) 2.10(6) 2.818(4) 167(5) yes O7 H14 O3 2 .68(6) 2.02(6) 2.682(4) 168(5) yes N1 H1 O2 3_566 .90 2.32 3.180(4) 158.9 yes N2 H4 O6 4_565 .90 2.08 2.953(3) 162.1 yes N3 H10 O5 . .85 2.12 2.933(4) 159.7 yes N3 H11 O5 2_655 .85 2.10 2.920(4) 160.8 yes N3 H12 O7 . .85 2.11 2.841(4) 142.9 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O2 S1 N1 Cu 66.6(2) ? O3 S1 N1 Cu -172.4(2) ? O1 S1 N1 Cu -53.9(2) ? C1 Cu N1 S1 -101.4(2) ? C2 Cu N1 S1 -99.3(3) ? N2 Cu N1 S1 60.7(2) ? O7 Cu N1 S1 150.31(18) ? O4 S2 N2 Cu 165.16(17) ? O6 S2 N2 Cu 43.40(18) ? O5 S2 N2 Cu -74.94(16) ? C1 Cu N2 S2 15.9(3) ? N1 Cu N2 S2 -131.80(14) ? C2 Cu N2 S2 36.06(18) ? O7 Cu N2 S2 134.19(14) ? N1 Cu C1 C2 178.0(2) ? N2 Cu C1 C2 31.0(4) ? O7 Cu C1 C2 -82.5(3) ? Cu C1 C2 C3 105.9(3) yes N1 Cu C2 C1 -3.3(4) ? N2 Cu C2 C1 -162.3(2) ? O7 Cu C2 C1 105.9(3) ? C1 Cu C2 C3 -116.6(4) ? N1 Cu C2 C3 -119.9(3) ? N2 Cu C2 C3 81.0(3) ? O7 Cu C2 C3 -10.7(3) ? C1 C2 C3 N3 -129.7(4) yes Cu C2 C3 N3 -50.0(4) ? _journal_paper_doi 10.1107/S0108270100016218