#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100770.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_1100770 _chemical_formula_sum 'C6 H8 N Ni O5 P' _chemical_formula_weight 263.81 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.7980(13) _cell_length_b 10.1982(15) _cell_length_c 17.945(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1610.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 327 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 16.818 _exptl_crystal_description 'blocky' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 2.602 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7358 _diffrn_reflns_av_R_equivalents 0.1062 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1415 _reflns_number_gt 816 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1415 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.34085(11) 0.34372(9) 0.81005(5) 0.0190(3) Uani 1 1 d . . . P1 P 0.5409(2) 0.1536(2) 0.71157(10) 0.0185(5) Uani 1 1 d . . . O1 O 0.5196(5) 0.2198(4) 0.7871(2) 0.0169(13) Uani 1 1 d . . . O2 O 0.5260(6) 0.0058(5) 0.7138(3) 0.0255(14) Uani 1 1 d . . . O3 O 0.6885(5) 0.1920(4) 0.6739(2) 0.0159(13) Uani 1 1 d . . . O4 O 0.3032(6) 0.3217(5) 0.6889(3) 0.0307(15) Uani 1 1 d . . . H4 H 0.215(9) 0.309(7) 0.666(4) 0.043 Uiso 1 1 d . . . N1 N 0.3848(6) 0.1601(7) 0.4236(3) 0.0168(14) Uani 1 1 d . . . C1 C 0.3306(10) 0.0672(8) 0.4697(4) 0.035(2) Uani 1 1 d . . . H1A H 0.2951 -0.0101 0.4483 0.042 Uiso 1 1 calc R . . C2 C 0.3237(10) 0.0775(9) 0.5449(4) 0.039(2) Uani 1 1 d . . . H2A H 0.2830 0.0102 0.5736 0.046 Uiso 1 1 calc R . . C3 C 0.3788(9) 0.1908(9) 0.5781(4) 0.030(2) Uani 1 1 d . . . C4 C 0.4366(10) 0.2875(8) 0.5325(5) 0.038(2) Uani 1 1 d . . . H4A H 0.4744 0.3650 0.5526 0.046 Uiso 1 1 calc R . . C5 C 0.4374(10) 0.2674(8) 0.4568(5) 0.034(2) Uani 1 1 d . . . H5A H 0.4775 0.3332 0.4268 0.041 Uiso 1 1 calc R . . C6 C 0.3740(9) 0.2061(8) 0.6602(4) 0.032(2) Uani 1 1 d . . . H6A H 0.3001 0.1385 0.6742 0.038 Uiso 1 1 calc R . . O1W O 0.1602(7) 0.4649(5) 0.8289(3) 0.0284(14) Uani 1 1 d G . . H1WA H 0.0963 0.4605 0.7900 0.040 Uiso 1 1 d G . . H1WB H 0.2050 0.5421 0.8394 0.040 Uiso 1 1 d G . . 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 Ni1 0.0242(6) 0.0167(5) 0.0161(5) -0.0002(5) -0.0003(5) 0.0012(5) P1 0.0209(12) 0.0192(11) 0.0154(10) 0.0000(10) -0.0016(9) 0.0021(11) O1 0.015(3) 0.022(3) 0.014(3) -0.002(2) 0.003(2) 0.001(2) O2 0.026(3) 0.012(3) 0.038(3) -0.007(2) 0.016(3) -0.004(2) O3 0.024(3) 0.004(3) 0.020(3) -0.002(2) 0.005(2) -0.002(2) O4 0.035(4) 0.027(3) 0.030(3) -0.004(3) -0.011(3) 0.006(3) N1 0.016(4) 0.013(3) 0.021(3) 0.000(3) -0.002(3) -0.002(3) C1 0.045(6) 0.033(6) 0.027(5) -0.002(4) -0.011(5) -0.014(5) C2 0.036(6) 0.056(7) 0.024(5) 0.008(5) -0.009(5) -0.014(5) C3 0.027(6) 0.036(6) 0.026(5) -0.001(4) 0.004(4) 0.023(4) C4 0.057(7) 0.023(5) 0.034(5) -0.016(4) -0.014(5) 0.002(5) C5 0.039(6) 0.024(5) 0.039(6) 0.009(4) -0.008(5) -0.005(5) C6 0.036(6) 0.029(5) 0.030(5) -0.004(4) -0.011(4) 0.007(4) O1W 0.031(4) 0.022(3) 0.032(4) -0.005(3) -0.011(3) -0.001(3)