#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012914.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_2012914 loop_ _publ_author_name 'Kuratieva, Natalia V.' 'Naumova, Marina I.' 'Naumov, Dmitry Yu.' _publ_section_title ; Hexaaquacobalt(II) bis(hypophosphite) and hexaaquacobalt(II)/nickel(II) bis(hypophosphite) ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i129 _journal_page_last i131 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Co0.5 Ni0.5 (H2 O)6] (H2 P O2)2' _chemical_formula_moiety '[Co0.5 Ni0.5 (H2 O)6] (H2 P O2)2' _chemical_formula_structural '[Co0.5 Ni0.5 (H2 O)6] (H2 P O2)2' _chemical_formula_sum 'Co0.5 H16 Ni0.5 O10 P2' _chemical_formula_weight 296.89 _chemical_name_common ; hexaaquacobalt(II)/nickel(II) hypophosphite ; _chemical_name_systematic ; hexaaquacobalt(II)/nickel(II) (0.5/0.5) bis(hypophosphite) ; _space_group_IT_number 142 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-I 4bd 2c' _symmetry_space_group_name_H-M 'I 41/a c d :2' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.3111(13) _cell_length_b 10.3111(13) _cell_length_c 20.346(3) _cell_measurement_reflns_used 24 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.08 _cell_measurement_theta_min 9.72 _cell_volume 2163.2(5) _computing_cell_refinement CD4CA0 _computing_data_collection 'CD4CA0 (Enraf-Nonius, 1989)' _computing_data_reduction 'CADDAT (Enraf-Nonius, 1989)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method 2\q/\q _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 0.016 _diffrn_reflns_av_sigmaI/netI 0.014 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1187 _diffrn_reflns_theta_full 27.46 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_min 3.44 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.014 _exptl_absorpt_correction_T_max 0.317 _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(CADDAT; Enraf-Nonius, 1989)' _exptl_crystal_colour 'light green' _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedron _exptl_crystal_F_000 1228 _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.63 _exptl_crystal_size_min 0.57 _refine_diff_density_max 0.23 _refine_diff_density_min -0.19 _refine_ls_extinction_coef 0.0030(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 49 _refine_ls_number_reflns 621 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.033 _refine_ls_R_factor_gt 0.021 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.3503P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.067 _refine_ls_wR_factor_ref 0.073 _reflns_number_gt 407 _reflns_number_total 621 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file av1112.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'I 41/a c d' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). '_geom_bond_publ_flag' value 'No' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (5 times). '_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). '_geom_angle_publ_flag' value 'No' changed to 'no' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times). '_geom_hbond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012914 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'y+1/4, x+1/4, z+1/4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Co1 0.0000 0.2500 0.1250 0.0293(2) Uani d SP 0.50 Co Ni1 0.0000 0.2500 0.1250 0.0293(2) Uani d SP 0.50 Ni P1 0.24135(6) 0.0000 0.2500 0.0319(2) Uani d S 1 P O1 0.16368(12) 0.08744(12) 0.29460(5) 0.0349(4) Uani d . 1 O H1 0.3229(16) -0.0665(17) 0.2876(7) 0.023(4) Uiso d . 1 H O1W 0.0000 0.2500 0.22614(10) 0.0516(6) Uani d S 1 O H1W 0.049(3) 0.200(2) 0.2487(15) 0.071(8) Uiso d . 1 H O2W 0.00205(18) 0.05080(15) 0.12382(10) 0.0548(5) Uani d . 1 O H2W 0.048(2) 0.014(2) 0.1409(8) 0.033(6) Uiso d . 1 H H3W -0.052(2) 0.015(2) 0.1052(9) 0.048(7) Uiso d . 1 H 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 Co1 0.0286(2) 0.0286(2) 0.0308(3) -0.00289(14) 0.000 0.000 Ni1 0.0286(2) 0.0286(2) 0.0308(3) -0.00289(14) 0.000 0.000 P1 0.0254(5) 0.0357(6) 0.0346(4) 0.000 0.000 -0.0102(2) O1 0.0337(7) 0.0355(7) 0.0355(6) 0.0003(5) 0.0017(5) -0.0104(5) O1W 0.054(2) 0.068(2) 0.0326(10) 0.0296(11) 0.000 0.000 O2W 0.0648(11) 0.0279(8) 0.0718(10) -0.0053(7) -0.0441(8) 0.0039(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 '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' P P 0.1023 0.0942 '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' 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 O1W Co1 O2W . . 90.67(5) yes O1W Co1 O2W . 8 89.33(5) yes O2W Co1 O2W . 8 88.83(10) yes O2W Co1 O2W . 10_454 178.66(11) no O2W Co1 O2W . 15_444 91.19(10) no O2W Co1 O2W 8 15_444 178.66(11) no O1W Ni1 O2W . . 90.67(5) no O1W Ni1 O2W . 8 89.33(5) no O2W Ni1 O2W . 8 88.83(10) no O2W Ni1 O2W . 10_454 178.66(11) no O2W Ni1 O2W . 15_444 91.19(10) no O2W Ni1 O2W 8 15_444 178.66(11) no O1 P1 O1 6 . 115.90(11) yes H1 P1 H1 6 . 101.4(15) no H1W O1W H1W 10_454 . 115(4) no H2W O2W H3W . . 119(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Co1 O1W 2.058(2) yes Co1 O2W 2.0542(16) yes Ni1 O1W 2.058(2) no Ni1 O2W 2.0542(16) no P1 O1 1.5092(12) yes P1 H1 1.328(15) yes O1W H1W 0.86(3) no O2W H2W 0.70(2) no O2W H3W 0.77(2) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1W H1W O1 . 0.86(3) 1.90(3) 2.7565(16) 177(3) yes O2W H2W O1 6 0.70(2) 2.06(2) 2.750(2) 170(2) yes O2W H3W O1 24 0.77(2) 1.98(2) 2.735(2) 168(2) yes