#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/39/2013921.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_2013921 loop_ _publ_author_name 'Naumova, Marina I.' 'Kuratieva, Natalia V.' 'Podberezskaya, Nina V.' 'Naumov, Dmitry Yu.' _publ_section_title ; The alkali hypophosphites KH~2~PO~2~, RbH~2~PO~2~ and CsH~2~PO~2~ ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i53 _journal_page_last i55 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'Rb H2 P O2' _chemical_formula_moiety 'H2 O2 P , Rb' _chemical_formula_structural 'Rb H2 P O2' _chemical_formula_sum 'H2 O2 P Rb' _chemical_formula_weight 150.46 _chemical_name_common 'Rubidium hypophosphite' _chemical_name_systematic ; Rubidium hypophosphite ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.9835(9) _cell_length_b 6.3678(7) _cell_length_c 7.5755(11) _cell_measurement_reflns_used 24 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 14.23 _cell_measurement_theta_min 9.91 _cell_volume 385.12(8) _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 298(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _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 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 732 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 24.89 _diffrn_reflns_theta_min 3.71 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 13.062 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_correction_T_min 0.095 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(CADDAT; Enraf-Nonius, 1989)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.595 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.577 _refine_diff_density_min -0.584 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 27 _refine_ls_number_reflns 366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.962 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0232 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.026P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.0567 _reflns_number_gt 289 _reflns_number_total 366 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bc1035.cif _[local]_cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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). 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 'Orthorhombic' changed to 'orthorhombic' 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_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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2013921 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Rb 0.63134(9) 0.2500 0.13795(8) 0.0322(3) Uani d S 1 . . Rb P 0.3847(3) 0.7500 0.3289(2) 0.0343(4) Uani d S 1 . . P H1 0.491(10) 0.7500 0.437(8) 0.041 Uiso d S 1 . . H H2 0.255(9) 0.7500 0.439(9) 0.041 Uiso d S 1 . . H O 0.3797(5) 0.5504(4) 0.2297(4) 0.0434(8) Uani d . 1 . . O 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 Rb 0.0286(4) 0.0313(4) 0.0368(4) 0.000 -0.0015(4) 0.000 P 0.0356(10) 0.0335(8) 0.0336(9) 0.000 0.0024(10) 0.000 O 0.0471(19) 0.0297(15) 0.0533(19) 0.000(2) 0.0100(19) -0.0003(15) 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 Rb O . 2.859(3) yes Rb O 4 2.932(3) yes Rb O 7_565 2.859(3) ? Rb O 6_656 2.932(3) ? Rb O 3_645 3.063(3) yes Rb O 5_665 3.063(3) ? P O . 1.478(3) yes P O 7_575 1.478(3) ? P H1 . 1.18(7) yes P H2 . 1.33(7) yes O Rb 6_556 2.932(3) ? O Rb 5_665 3.063(3) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 '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 O Rb O . 7_565 83.96(13) ? O Rb O . 6_656 87.46(7) ? O Rb O . 4 145.93(3) ? O Rb O 7_565 6_656 145.93(3) ? O Rb O 7_565 4 87.46(7) ? O Rb O 6_656 4 81.44(12) ? O Rb O 7_565 3_645 85.58(9) ? O Rb O . 3_645 118.58(6) ? O Rb O 6_656 3_645 126.97(7) ? O Rb O 4 3_645 93.43(6) ? O Rb O 7_565 5_665 118.58(6) ? O Rb O . 5_665 85.58(9) ? O Rb O 6_656 5_665 93.43(6) ? O Rb O 4 5_665 126.97(7) ? O Rb O 3_645 5_665 49.05(10) ? O P O . 7_575 118.7(3) yes O P H1 . . 111.9(13) yes O P H1 7_575 . 111.9(13) ? O P H2 . . 107.4(13) yes O P H2 7_575 . 107.4(13) ? H1 P H2 . . 97(4) yes P O Rb . . 132.9(2) ? P O Rb . 6_556 113.91(18) ? Rb O Rb . 6_556 97.00(8) ? P O Rb . 5_665 96.11(13) ? Rb O Rb . 5_665 94.42(9) ? Rb O Rb 6_556 5_665 124.22(12) ? _cod_database_fobs_code 2013921 _journal_paper_doi 10.1107/S0108270104002409