#------------------------------------------------------------------------------ #$Date: 2012-02-26 23:34:47 +0200 (Sun, 26 Feb 2012) $ #$Revision: 35909 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/68/7106863.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_7106863 loop_ _publ_author_name 'Bani Kanta Sarma' 'Muhammed Yousufuddin' 'Thomas Kodadek' _publ_section_title ; Acyl hydrazides as peptoid sub-monomers ; _journal_name_full Chem.Commun. _journal_page_first 10590 _journal_volume 47 _journal_year 2011 _chemical_formula_sum 'C6 H11 N3 O3' _chemical_formula_weight 173.18 _chemical_name_systematic ; ? ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 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 97.832(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 4.7784(18) _cell_length_b 10.846(4) _cell_length_c 8.480(3) _cell_measurement_reflns_used 2044 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.89 _cell_measurement_theta_min 2.42 _cell_volume 435.4(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0961 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 4310 _diffrn_reflns_theta_full 28.37 _diffrn_reflns_theta_max 28.37 _diffrn_reflns_theta_min 2.42 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 184 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.282 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 2131 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0564 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1328 _refine_ls_wR_factor_ref 0.1440 _reflns_number_gt 1720 _reflns_number_total 2131 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c1cc12750k.txt _[local]_cod_data_source_block compd1d_ _[local]_cod_cif_authors_sg_H-M P2(1) _cod_database_code 7106863 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -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 C1 C 0.3987(7) 0.9159(2) 0.8431(3) 0.0620(7) Uani 1 1 d . H1A H 0.2724 0.9851 0.8306 0.093 Uiso 1 1 calc R H1B H 0.5707 0.9366 0.8026 0.093 Uiso 1 1 calc R H1C H 0.4401 0.8952 0.9540 0.093 Uiso 1 1 calc R C2 C 0.2630(5) 0.8079(2) 0.7532(2) 0.0410(5) Uani 1 1 d . C3 C 0.3490(5) 0.5595(2) 0.5624(3) 0.0405(5) Uani 1 1 d . C4 C 0.5687(6) 0.5377(3) 0.7024(3) 0.0620(7) Uani 1 1 d . H4A H 0.5018 0.5677 0.7971 0.093 Uiso 1 1 calc R H4B H 0.7388 0.5805 0.6872 0.093 Uiso 1 1 calc R H4C H 0.6067 0.4510 0.7131 0.093 Uiso 1 1 calc R C5 C 0.0357(4) 0.7038(2) 0.4032(2) 0.0388(4) Uani 1 1 d . H5A H -0.0565 0.7797 0.4279 0.047 Uiso 1 1 calc R H5B H -0.1029 0.6381 0.3976 0.047 Uiso 1 1 calc R C6 C 0.1400(4) 0.71685(19) 0.2417(2) 0.0356(4) Uani 1 1 d . N1 N 0.3798(4) 0.77437(15) 0.6228(2) 0.0388(4) Uani 1 1 d . H1 H 0.5246 0.8131 0.5980 0.047 Uiso 1 1 calc R N2 N 0.2637(4) 0.67700(16) 0.5295(2) 0.0387(4) Uani 1 1 d . N3 N -0.0633(4) 0.7295(2) 0.1210(2) 0.0537(6) Uani 1 1 d . H3A H -0.0221 0.7388 0.0261 0.064 Uiso 1 1 calc R H3B H -0.2371 0.7284 0.1371 0.064 Uiso 1 1 calc R O1 O 0.0669(4) 0.75037(19) 0.7960(2) 0.0638(5) Uani 1 1 d . O2 O 0.2423(4) 0.47525(16) 0.4763(2) 0.0548(5) Uani 1 1 d . O3 O 0.3914(3) 0.71726(17) 0.23009(19) 0.0502(4) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0844(19) 0.0489(14) 0.0518(13) -0.0116(11) 0.0062(13) -0.0056(13) C2 0.0492(12) 0.0420(11) 0.0316(9) 0.0011(8) 0.0052(8) 0.0001(9) C3 0.0461(10) 0.0349(10) 0.0423(10) 0.0006(8) 0.0128(9) -0.0007(9) C4 0.0704(15) 0.0480(14) 0.0629(16) 0.0086(12) -0.0079(13) 0.0033(12) C5 0.0352(9) 0.0493(11) 0.0327(8) 0.0002(9) 0.0075(7) 0.0031(9) C6 0.0352(9) 0.0369(10) 0.0365(9) -0.0014(8) 0.0114(7) -0.0014(8) N1 0.0458(9) 0.0338(9) 0.0382(8) -0.0022(7) 0.0109(7) -0.0052(7) N2 0.0444(9) 0.0378(9) 0.0329(8) -0.0028(6) 0.0019(7) 0.0018(7) N3 0.0367(9) 0.0902(17) 0.0359(8) 0.0114(10) 0.0113(7) -0.0013(10) O1 0.0720(11) 0.0784(13) 0.0455(9) -0.0059(9) 0.0244(8) -0.0205(10) O2 0.0617(10) 0.0413(9) 0.0621(10) -0.0099(8) 0.0102(8) -0.0047(7) O3 0.0333(7) 0.0679(11) 0.0515(8) 0.0034(8) 0.0134(6) 0.0003(8) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 H1A 109.5 C2 C1 H1B 109.5 H1A C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 O1 C2 N1 121.6(2) O1 C2 C1 123.0(2) N1 C2 C1 115.3(2) O2 C3 N2 119.0(2) O2 C3 C4 122.8(2) N2 C3 C4 118.1(2) C3 C4 H4A 109.5 C3 C4 H4B 109.5 H4A C4 H4B 109.5 C3 C4 H4C 109.5 H4A C4 H4C 109.5 H4B C4 H4C 109.5 N2 C5 C6 112.15(16) N2 C5 H5A 109.2 C6 C5 H5A 109.2 N2 C5 H5B 109.2 C6 C5 H5B 109.2 H5A C5 H5B 107.9 O3 C6 N3 124.52(17) O3 C6 C5 121.27(18) N3 C6 C5 114.20(15) C2 N1 N2 119.48(18) C2 N1 H1 120.3 N2 N1 H1 120.3 C3 N2 N1 120.79(18) C3 N2 C5 121.03(17) N1 N2 C5 118.04(18) C6 N3 H3A 120.0 C6 N3 H3B 120.0 H3A N3 H3B 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.497(3) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C2 O1 1.221(3) C2 N1 1.354(3) C3 O2 1.235(3) C3 N2 1.356(3) C3 C4 1.492(3) C4 H4A 0.9600 C4 H4B 0.9600 C4 H4C 0.9600 C5 N2 1.449(3) C5 C6 1.526(3) C5 H5A 0.9700 C5 H5B 0.9700 C6 O3 1.218(2) C6 N3 1.319(3) N1 N2 1.389(2) N1 H1 0.8600 N3 H3A 0.8600 N3 H3B 0.8600