#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/18/2101878.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_2101878 loop_ _publ_author_name 'Soma Ghosh' 'Monika Mukherjee' 'Alpana Seal' 'Siddhartha Ray' _publ_section_title ; X-ray Study of M^II^(ClO~4~)~2~.6H~2~O (M^II^ = Zn, Ni): Twinning, Disorder and Phase Transitions ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 639 _journal_page_last 644 _journal_paper_doi 10.1107/S010876819700195X _journal_volume 53 _journal_year 1997 _chemical_formula_analytical 'H12 Cl2 O14 Zn' _chemical_formula_moiety 'H12 Cl2 O14 Zn' _chemical_formula_structural 'H12 Cl2 O14 Zn' _chemical_formula_sum 'Cl2 H12 O14 Zn' _chemical_formula_weight 372.37 _chemical_name_systematic ; Zinc perchlorate hexahydrate ; _space_group_IT_number 186 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 6c -2c' _symmetry_space_group_name_H-M 'P 63 m c' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 1 _cell_length_a 7.7959(4) _cell_length_b 7.7959(4) _cell_length_c 5.3033(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 10 _cell_volume 279.13(3) _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 594 _diffrn_reflns_theta_max 24.90 _diffrn_reflns_theta_min 3.02 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.751 _exptl_absorpt_correction_type none _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method none _exptl_crystal_description Prism _exptl_crystal_F_000 188 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.299 _refine_diff_density_min -0.730 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.04(8) _refine_ls_extinction_coef 0.09(4) _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_goodness_of_fit_all 1.211 _refine_ls_goodness_of_fit_obs 1.212 _refine_ls_hydrogen_treatment 'H atoms refined isotropically' _refine_ls_matrix_type full _refine_ls_number_parameters 26 _refine_ls_number_reflns 115 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.211 _refine_ls_restrained_S_obs 1.212 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_obs 0.0380 _refine_ls_shift/esd_max 0.567 _refine_ls_shift/esd_mean 0.202 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.16P], where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1071 _refine_ls_wR_factor_obs 0.1065 _reflns_number_observed 114 _reflns_number_total 115 _reflns_observed_criterion >2sigma(I) _cod_data_source_file li0238.cif _cod_data_source_block zinc _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.16P], where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.16P], where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 63 mc' _cod_original_formula_sum 'H12 Cl2 O14 Zn' _cod_database_code 2101878 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z+1/2' 'x-y, -y, z+1/2' '-x, -x+y, z+1/2' 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 Zn 0.0300(10) 0.0300(10) 0.048(2) 0.0150(10) 0.000 0.000 Cl 0.0300(10) 0.0300(10) 0.053(2) 0.0150(10) 0.000 0.000 O1 0.076(5) 0.076(5) 0.040(9) 0.038(3) 0.000 0.000 O2 0.066(3) 0.066(4) 0.076(5) 0.045(3) 0.005(2) -0.005(2) OW 0.048(2) 0.048(2) 0.074(4) 0.030(2) 0.001(2) -0.001(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Zn 0.0000 0.0000 0.2500 0.0360(10) Uani d SP 0.50 Zn Cl 0.3333 0.6667 0.0062(12) 0.0380(10) Uani d S 1 Cl O1 0.3333 0.6667 0.280(3) 0.064(4) Uani d S 1 O O2 0.4320(4) 0.5680(4) -0.0869(16) 0.064(3) Uani d S 1 O OW 0.1242(4) 0.8758(4) 0.504(2) 0.054(2) Uani d S 1 O H 0.100(10) 0.750(10) 0.47(3) 0.09(3) Uiso d . 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag OW Zn OW 4_564 5_444 86.3(4) yes OW Zn OW 4_564 1_545 179.0(5) yes OW Zn OW 5_444 1_545 94.40(10) yes OW Zn OW 1_545 2_665 84.9(3) yes O2 Cl O2 3_565 2_665 108.5(2) no O2 Cl O2 3_565 . 108.5(2) no O2 Cl O2 2_665 . 108.5(2) yes O2 Cl O1 . . 110.3(5) yes O2 Cl O1 3_565 . 110.3(5) no O2 Cl O1 2_665 . 110.3(5) no 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 Zn OW 4_564 2.123(7) yes Zn OW 5_444 2.123(7) no Zn OW 6_654 2.123(7) no Zn OW 1_545 2.152(7) yes Zn OW 2_665 2.152(7) no Zn OW 3_455 2.152(7) no Cl O1 . 1.450(15) yes Cl O2 . 1.421(5) yes Cl O2 3_565 1.421(5) no Cl O2 2_665 1.421(5) no OW H . 0.92(9) yes