Syntheses, Structures, and Magnetic Properties of Metal(II) Phosphates with M(OH)(PO4)2- Layers (M = Ni, Co, Mg)
Nobuaki Hamanaka; Hideo Imoto; Inorganic Chemistry 37 (1998) 5844–5850; doi:10.1021/ic980595n

data_4323132
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of Metal(II) Phosphates
 with M(OH)(PO4)2- Layers (M = Ni, Co, Mg)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5844
_journal_page_last               5850
_journal_paper_doi               10.1021/ic980595n
_journal_volume                  37
_journal_year                    1998
_chemical_formula_structural     'Na (H3O)2 (Ni4 (OH)4 (HPO4)3 (H2PO4))'
_chemical_formula_sum            'H15 Na Ni4 O22 P4'
_chemical_formula_weight         748.76
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           'Int. Tables Vol IV Tables 2.2B'
_cell_angle_alpha                90
_cell_angle_beta                 106.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.374(2)
_cell_length_b                   12.811(4)
_cell_length_c                   8.407(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    296
_cell_measurement_theta_max      15.7
_cell_measurement_theta_min      13.8
_cell_volume                     866.1(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_structure_refinement  'ANYBLK(Imoto, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           Mo_K\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7942
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        0.20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.794
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y-scan method (North & Phillops, 1968)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             748.00
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.404
_refine_diff_density_min         -0.987
_refine_ls_abs_structure_details
;
  Reflections hkl and -h-k-l were not averaged.The crystal was assumed to 
  contain both of the enantiomorphs and the ratio was refined by Flack's 
  method (Flack, H. D. Acta Cryst. A39, 876).
;
_refine_ls_abs_structure_Flack   0.72(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.248
_refine_ls_goodness_of_fit_obs   1.306
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_constraints    1
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3139
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_obs          0.0688
_refine_ls_shift/esd_max         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0079|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0935
_refine_ls_wR_factor_obs         0.0865
_reflns_number_observed          3139
_reflns_number_total             3972
_reflns_observed_criterion       >1.0sigma(I)
_cod_data_source_file            ic980595n_1.cif
_cod_data_source_block           1_Na(H3O)2{Ni4(OH)4(HPO4)3(H2PO4)}
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.0079|Fo|^2^]' 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) + 0.0079|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'H15 Na O22 Ni4 P4 '
_cod_database_code               4323132