#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003320.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_2003320 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 621 _journal_page_last 623 _publ_section_title ; An Aminobenzyldioxocyclam Nickel(II) Complex ; _chemical_formula_sum 'C17 H25 N5 Ni O2' _chemical_formula_weight 390.13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _symmetry_space_group_name_H-M 'P m n 21' _cell_length_a 9.415(3) _cell_length_b 8.103(2) _cell_length_c 11.957(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 912.2(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 18.5 _exptl_absorpt_coefficient_mu 1.084 _cell_measurement_temperature 130(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_colour yellow _chemical_compound_source ? _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \w _exptl_absorpt_correction_type 'XABS (Hope & Moezzi, 1994)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.86 _diffrn_reflns_number 1796 _reflns_number_total 1272 _reflns_number_observed 1134 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 1 _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0291 _refine_ls_wR_factor_obs 0.0667 _refine_ls_wR_factor_all 0.0709 _refine_ls_goodness_of_fit_obs 1.024 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_number_reflns 1272 _refine_ls_number_parameters 124 _refine_ls_hydrogen_treatment ; H atoms riding with C---H = 0.96 and N---H = 0.94\%A ; _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0388P)^2^] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.017 _refine_diff_density_max 0.262 _refine_diff_density_min -0.245 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'Ni' 'Ni' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3393 1.1 _refine_ls_abs_structure_Flack -0.01(2) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni 1 0 0.63340(6) 0.02252(6) 0.02670(14) O1 1 0.2444(4) 0.6394(3) 0.3011(3) 0.0662(10) N1 1 0.1442(6) 0.6147(4) 0.1284(4) 0.0386(11) N2 1 0.1493(5) 0.6418(4) -0.0873(3) 0.0318(10) H2C 1 0.1560(5) 0.5347(4) -0.1170(3) 0.045 N3 1 0 1.2000(6) -0.1284(5) 0.067(2) H3A 1 -0.0881 1.2150(6) -0.1675(5) 0.045 C1 1 0.1378(5) 0.6460(5) 0.2371(3) 0.0456(10) C2 1 0.2816(4) 0.5796(5) 0.0782(4) 0.0492(11) H2A 1 0.2932(4) 0.4638(5) 0.0637(4) 0.045 H2B 1 0.3571(4) 0.6152(5) 0.1264(4) 0.045 C3 1 0.2856(4) 0.6737(5) -0.0299(4) 0.0472(11) H3C 1 0.2950(4) 0.7896(5) -0.0151(4) 0.045 H3D 1 0.3641(4) 0.6392(5) -0.0756(4) 0.045 C4 1 0.1339(4) 0.7518(5) -0.1857(3) 0.0432(9) H4A 1 0.2154(4) 0.7400(5) -0.2333(3) 0.045 H4B 1 0.1304(4) 0.8641(5) -0.1603(3) 0.045 C5 1 0 0.7172(9) -0.2505(6) 0.051(2) H5A 1 0 0.6025(9) -0.2706(6) 0.045 H5B 1 0 0.7807(9) -0.3182(6) 0.045 C6 1 0 0.7012(7) 0.2877(5) 0.045(2) H6A 1 0 0.6565(7) 0.3621(5) 0.045 C7 1 0 0.8929(6) 0.3001(5) 0.053(2) H7A 1 0.0824 0.9251(6) 0.3421(5) 0.045 C8 1 0 0.9841(6) 0.1907(4) 0.0448(13) C9 1 0.1252(4) 1.0244(4) 0.1380(3) 0.0449(9) H9A 1 0.2135(4) 1.0002(4) 0.1747(3) 0.045 C10 1 0.1266(4) 1.0999(4) 0.0327(5) 0.0495(10) H10A 1 0.2149(4) 1.1232(4) -0.0041(5) 0.045 C11 1 0 1.1372(6) -0.0198(5) 0.0470(13) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ni 0.0242(2) 0.000 0.000 0.0291(2) -0.0002(4) 0.0269(2) O1 0.096(3) 0.005(2) -0.047(2) 0.046(2) 0.000(2) 0.056(2) N1 0.039(3) 0.0023(15) -0.007(2) 0.038(2) -0.0042(15) 0.039(2) N2 0.025(2) -0.0017(13) 0.005(2) 0.034(2) -0.0051(13) 0.037(2) N3 0.081(4) 0.000 0.000 0.063(3) 0.023(3) 0.055(3) C1 0.069(3) 0.002(2) -0.020(2) 0.030(2) 0.001(2) 0.038(2) C2 0.034(2) 0.004(2) -0.016(2) 0.052(2) -0.006(3) 0.062(3) C3 0.021(2) -0.008(2) 0.003(2) 0.057(2) -0.019(3) 0.064(3) C4 0.048(2) -0.006(2) 0.013(2) 0.041(2) 0.000(2) 0.041(2) C5 0.073(5) 0.000 0.000 0.051(4) 0.004(3) 0.029(3) C6 0.083(5) 0.000 0.000 0.028(3) 0.004(3) 0.024(3) C7 0.088(5) 0.000 0.000 0.038(3) -0.008(2) 0.032(2) C8 0.075(4) 0.000 0.000 0.022(2) -0.007(2) 0.038(3) C9 0.058(2) -0.007(2) -0.010(2) 0.031(2) -0.004(2) 0.046(2) C10 0.057(2) -0.0099(14) -0.002(3) 0.034(2) -0.003(2) 0.058(3) C11 0.067(3) 0.000 0.000 0.029(2) -0.004(2) 0.045(3) _cod_database_code 2003320