Synthesis, Structure, and Spectroscopy of Rare Earth Hypophosphites. 1. Anhydrous and Monohydrated Lanthanide Hypophosphites
Peter A. Tanner; Michele D. Faucher; Thomas C. W. Mak; Inorganic Chemistry 38 (1999) 6008–6023; doi:10.1021/ic990187z

data_4322540
_publ_section_title
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 Synthesis, Structure, and Spectroscopy of Rare Earth Hypophosphites. 1.
 Anhydrous and Monohydrated Lanthanide Hypophosphites
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6008
_journal_page_last               6023
_journal_paper_doi               10.1021/ic990187z
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         La(H2PO2)3.H2O
_chemical_formula_sum            'C0 H8 La O7 P3'
_chemical_formula_weight         351.88
_chemical_name_common            'lanthanum(III) hypophosphite hydrate'
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.57(2)
_cell_angle_beta                 98.26(1)
_cell_angle_gamma                104.35(1)
_cell_formula_units_Z            2
_cell_length_a                   7.229(1)
_cell_length_b                   7.983(1)
_cell_length_c                   8.934(2)
_cell_measurement_temperature    293(2)
_cell_volume                     452.26(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8576
_diffrn_reflns_theta_full        47.62
_diffrn_reflns_theta_max         47.62
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    5.246
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.701
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0016(7)
_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   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         8504
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.4372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                7847
_reflns_number_total             8504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990187z_2.cif
_cod_data_source_block           lahpw
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.4372P] 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^)+(0.0340P)^2^+0.4372P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        452.3(1)
_cod_database_code               4322540