#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308329.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_4308329 loop_ _publ_author_name 'Simona Marincean' 'Radu Custelcean' 'Robin S. Stein' 'James E. Jackson' _publ_section_title ; Structural Reinvestigation of Ammonium Hypophosphite: Was Dihydrogen Bonding Observed Long Ago? ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 45 _journal_page_last 48 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'H6 N O2 P' _chemical_formula_weight 83.03 _chemical_name_common NH4-H2PO2 _chemical_name_systematic ; ? ; _space_group_IT_number 67 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2a 2' _symmetry_space_group_name_H-M 'C m m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.5192(18) _cell_length_b 7.4977(12) _cell_length_c 3.9607(6) _cell_measurement_temperature 173(2) _cell_volume 342.08(9) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Siemens SMART CCD' _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 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 1508 _diffrn_reflns_theta_full 28.29 _diffrn_reflns_theta_max 28.29 _diffrn_reflns_theta_min 3.54 _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_type empirical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 176 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.284 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef 0.037(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.237 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 22 _refine_ls_number_reflns 236 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.237 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0198 _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^)+(0.0358P)^2^+0.1620P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.0611 _reflns_number_gt 225 _reflns_number_total 236 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048657zsi20040924_040917.cif _[local]_cod_data_source_block amhypo _cod_database_code 4308329 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.0000 0.2500 0.05195(13) 0.0145(3) Uani 1 4 d S . . HP H 0.0000 0.113(3) 0.259(5) 0.024(5) Uiso 1 2 d S . . O O 0.11255(9) 0.2500 -0.1404(3) 0.0228(4) Uani 1 2 d S . . N N 0.2500 0.0000 0.5000 0.0199(4) Uani 1 4 d S . . HN H 0.2920(11) 0.065(3) 0.377(3) 0.029(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.0133(4) 0.0152(4) 0.0150(4) 0.000 0.000 0.000 O 0.0158(6) 0.0246(6) 0.0279(6) 0.000 0.0056(5) 0.000 N 0.0151(9) 0.0208(10) 0.0239(9) 0.000 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O P O 119.11(10) 2 . ? O P HP 108.5(4) 2 . ? O P HP 108.5(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P O 1.5038(11) 2 ? P O 1.5038(11) . ? P HP 1.31(2) . ? N HN 0.845(14) . ?