An ordered low-temperature phase of barium nitroprusside trihydrate studied by neutron diffraction
G. Chevrier; J.M. Kiat; J. Guida; A. Navaza; Acta Crystallographica Section C 59 (2003) i59–i62; doi:10.1107/S0108270103010199

data_2013520
_publ_section_title
;
 An ordered low-temperature phase of barium nitroprusside trihydrate
 studied by neutron diffraction
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i59
_journal_page_last               i62
_journal_paper_doi               10.1107/S0108270103010199
_journal_volume                  59
_journal_year                    2003
_chemical_formula_analytical     'C5 Ba1 Fe1 N6 O1, 3H2 O1'
_chemical_formula_iupac          'Ba [Fe (C N)5 (N O)], 3H2 O'
_chemical_formula_moiety         'Ba1 1+, C5 Fe1 N6 O1 1-, 3H2 O1'
_chemical_formula_structural     'C5 Ba1 Fe1 N6 O1, 3H2 O1'
_chemical_formula_sum            'C5 H6 Ba Fe N6 O4'
_chemical_formula_weight         407.31
_chemical_name_common            'baryum nitroprusside trihydrate'
_chemical_name_systematic        ?
_space_group_IT_number           1
_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
_cell_angle_alpha                90.040(3)
_cell_angle_beta                 90.003(5)
_cell_angle_gamma                89.994(5)
_cell_formula_units_Z            4
_cell_length_a                   19.01(9)
_cell_length_b                   7.694(16)
_cell_length_c                   8.72(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      15.5
_cell_volume                     1275(7)
_computing_molecular_graphics    'CAMERON (Pearce et al., 2000)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.739
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_device
'Four-circle diffractometer, 6T2 Orphee reactor'
_diffrn_measurement_method
;
\w 3<2\q<50
\w-\q 50<2\q<80
\w-2\q 80<2\q<110
;
_diffrn_radiation_monochromator  'Er filters'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'Orphee reactor'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.548(5)
_diffrn_reflns_av_R_equivalents  0.0070
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2453
_diffrn_reflns_theta_full        54.96
_diffrn_reflns_theta_max         54.96
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.1579
_exptl_absorpt_correction_T_max  0.7934
_exptl_absorpt_correction_T_min  0.4976
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'laboratory program'
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             419.0
_exptl_crystal_size_max          5.5
_exptl_crystal_size_mid          2.5
_exptl_crystal_size_min          1.5
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.092
_refine_ls_extinction_coef       0.00229(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   3.748
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         2415
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      3.745
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0782
_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^) where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0874
_reflns_number_observed          2260
_reflns_number_total             2415
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            sq1015.cif
_cod_data_source_block           I
_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 
;
_cod_original_cell_volume        1276.(7)
_cod_original_formula_sum        'C5 H6  Ba1 Fe1 N6 O4'
_cod_database_code               2013520