Structural Reinvestigation of Ammonium Hypophosphite: Was Dihydrogen Bonding Observed Long Ago?
Simona Marincean; Radu Custelcean; Robin S. Stein; James E. Jackson; Inorganic Chemistry 44 (2005) 45–48; doi:10.1021/ic048657z

data_4308329
_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_paper_doi               10.1021/ic048657z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'H6 N O2 P'
_chemical_formula_weight         83.03
_chemical_name_common            NH4-H2PO2
_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)
_cod_data_source_file            ic048657zsi20040924_040917.cif
_cod_data_source_block           amhypo
_cod_database_code               4308329