#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003611.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_2003611 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1059 _journal_page_last 1060 _publ_section_title ; Diaqua[2,13-dimethyl-3,12,18-triaza-6,9-dioxabicyclo[12.3.1]octadeca- 1(18),2,12,14,16-pentaene]magnesium(II) Diperchlorate ; _chemical_formula_sum 'C15 H25 Cl2 Mg N3 O12' _chemical_formula_weight 534.59 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.964(3) _cell_length_b 13.603(1) _cell_length_c 10.835(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.000(7) _cell_angle_gamma 90.00 _cell_volume 2335.5(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.370 _cell_measurement_temperature 298 _exptl_crystal_description octahedral _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.29 _exptl_crystal_colour yellow _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1589 _reflns_number_total 1526 _reflns_number_observed 1075 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 22.45 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0675 _refine_ls_wR_factor_obs 0.1700 _refine_ls_wR_factor_all 0.1994 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_number_reflns 1526 _refine_ls_number_parameters 157 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.1011P)^2^ + 6.6075P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.457 _refine_diff_density_min -0.342 _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 'Mg' 'Mg' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0486 0.0 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1484 0.1 _computing_structure_solution ; MULTAN80 (Main, Fiske, Hull, Lessinger, Germain, Declercq & Woolfson, 1980) ; 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 Cl 1 0.31683(10) 0.84307(13) 0.31915(15) 0.0561(6) Mg 1 0.5000 0.7231(2) 0.7500 0.0358(7) OW1 1 0.3988(3) 0.7266(3) 0.6112(4) 0.0546(12) O1 1 0.5487(3) 0.8514(3) 0.6615(4) 0.0638(13) O2 1 0.3896(4) 0.8505(5) 0.4039(6) 0.132(3) O3 1 0.2782(4) 0.7527(5) 0.3360(9) 0.145(3) O4 1 0.3389(5) 0.8529(7) 0.2031(6) 0.157(3) O5 1 0.2579(5) 0.9145(6) 0.3318(8) 0.155(3) N1 1 0.5000 0.5628(5) 0.7500 0.039(2) N2 1 0.5862(3) 0.6692(4) 0.6174(4) 0.0480(13) C1 1 0.5493(4) 0.5133(4) 0.6802(5) 0.047(2) C2 1 0.5509(5) 0.4111(5) 0.6790(7) 0.070(2) H2 1 0.5859(5) 0.3774(5) 0.6309(7) 0.105 C3 1 0.5000 0.3615(8) 0.7500 0.080(3) H3 1 0.5000 0.2931(8) 0.7500 0.120 C4 1 0.5990(4) 0.5781(5) 0.6059(6) 0.052(2) C5 1 0.6583(5) 0.5315(7) 0.5249(7) 0.084(3) H5A 1 0.6859(5) 0.5820(7) 0.4828(7) 0.125 H5B 1 0.6270(5) 0.4896(7) 0.4647(7) 0.125 H5C 1 0.6998(5) 0.4933(7) 0.5756(7) 0.125 C6 1 0.6275(5) 0.7440(7) 0.5495(7) 0.077(2) H6A 1 0.6873(5) 0.7294(7) 0.5545(7) 0.116 H6B 1 0.6042(5) 0.7426(7) 0.4626(7) 0.116 C7 1 0.6165(9) 0.8395(8) 0.5988(14) 0.160(6) H7A 1 0.6669(9) 0.8561(8) 0.6543(14) 0.239 H7B 1 0.6120(9) 0.8862(8) 0.5306(14) 0.239 C8 1 0.5296(8) 0.9411(6) 0.7103(13) 0.145(5) H8A 1 0.5812(8) 0.9685(6) 0.7535(13) 0.217 H8B 1 0.5109(8) 0.9848(6) 0.6418(13) 0.217 HW1 1 0.3507(36) 0.6981(56) 0.6130(75) 0.100 HW2 1 0.4041(51) 0.7700(49) 0.5567(64) 0.100 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 Cl 0.0470(10) -0.0003(8) 0.0026(7) 0.0675(12) 0.0047(8) 0.0530(10) Mg 0.0380(15) 0.000 0.0053(11) 0.0363(15) 0.000 0.0334(14) OW1 0.044(2) -0.006(2) 0.001(2) 0.067(3) 0.011(2) 0.051(3) O1 0.062(3) -0.009(2) 0.011(3) 0.049(3) 0.015(2) 0.081(3) O2 0.101(5) -0.065(4) -0.058(4) 0.151(6) 0.080(5) 0.124(5) O3 0.101(5) -0.045(4) -0.037(5) 0.108(5) 0.045(5) 0.213(9) O4 0.155(7) -0.008(7) 0.048(4) 0.257(10) -0.012(5) 0.066(4) O5 0.134(6) 0.071(6) 0.024(5) 0.171(7) -0.044(6) 0.161(7) N1 0.040(4) 0.000 0.003(3) 0.039(4) 0.000 0.038(4) N2 0.041(3) -0.003(3) 0.010(2) 0.065(4) 0.002(3) 0.039(3) C1 0.043(4) 0.003(3) -0.013(3) 0.047(4) -0.006(3) 0.045(4) C2 0.086(6) 0.022(4) -0.012(4) 0.053(5) -0.019(4) 0.066(5) C3 0.102(9) 0.000 -0.017(7) 0.051(7) 0.000 0.079(8) C4 0.038(3) 0.009(3) 0.002(3) 0.072(5) -0.022(3) 0.044(4) C5 0.059(4) 0.010(5) 0.016(4) 0.119(7) -0.037(5) 0.074(5) C6 0.067(5) -0.016(5) 0.022(4) 0.107(7) 0.017(5) 0.061(4) C7 0.208(13) -0.038(8) 0.159(12) 0.079(7) 0.016(8) 0.225(14) C8 0.201(14) -0.023(6) 0.091(10) 0.037(5) 0.000(6) 0.212(14) _cod_database_code 2003611