Crystal structure of zirconium phosphide sulphide, ZrP1.4S0.6
Andreas Schlechte; Katrin Meier; Rainer Niewa; Yurii Prots; Marcus Schmidt; Rüdiger Kniep; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 375–; doi:

data_8103035
_publ_section_title
;
 Crystal structure of zirconium phosphide sulphide, ZrP1.4S0.6
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              375
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'Zr P1.4 S0.6'
_chemical_formula_sum            'P1.4 S0.6 Zr'
_chemical_formula_weight         154.25
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_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            2
_cell_length_a                   3.5854(2)
_cell_length_b                   3.5854(2)
_cell_length_c                   7.8195(5)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      83.31
_cell_measurement_theta_min      22.75
_cell_volume                     100.520(10)
_computing_cell_refinement       'WinCSD (Akselrud, 1993) [9]'
_computing_data_collection       'CrystalClear, (Rigaku MSC, 2004)'
_computing_data_reduction        'CrystalClear, (Rigaku MSC, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997) [8]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [8]'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
scan:
 Number of images: 300
            Slice: -30.0000 - 210.0000
      Image width: 0.8000
         Exp time: 70.0000
    Rotation axis: Phi
            Omega: 0.0000
              Chi: 0.0000
              Phi: 0.0000
              XTD: 42.0800
           2theta: -25.0000
scan:
 Number of images: 70
            Slice: -38.0000 - 18.0000
      Image width: 0.8000
         Exp time: 70.0000
    Rotation axis: Omega
            Omega: 0.0000
              Chi: -90.0000
              Phi: 85.0000
              XTD: 42.0800
           2theta: -25.0000
;
_diffrn_measurement_device       'Rigaku AFC7'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       'Mercury70 CCD (2x2 bin mode)'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            756
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        33.51
_diffrn_reflns_theta_max         33.51
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    6.789
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'silver metallic'
_exptl_crystal_density_diffrn    5.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             142
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.178
_refine_ls_extinction_coef       0.021(5)
_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   1.173
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10
_refine_ls_number_reflns         145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.020
_refine_ls_R_factor_gt           0.018
_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^)+(0.0000P)^2^+0.2338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.032
_refine_ls_wR_factor_ref         0.033
_reflns_number_gt                135
_reflns_number_total             145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            710023.cff
_cod_data_source_block           km_024c
_cod_depositor_comments
;
The following corrections have been performed
in the original file before processing it for deposition
(the diff against the Z. Krist. - NCS original is given):

Index: 2009/03/710023.cff
===================================================================
--- 2009/03/710023.cff    (revision 562)
+++ 2009/03/710023.cff    (revision 563)
@@ -208,8 +208,8 @@
 ; 
 _chemical_name_common             ? 
 _chemical_melting_point           ? 
-_chemical_formula_moiety      'ZrP~1.4~Se~0.6~'
-_chemical_formula_sum              ?
+_chemical_formula_moiety      'Zr P1.4 Se0.6'
+_chemical_formula_sum         'Zr P1.4 Se0.6'
 _chemical_formula_weight      154.25 
  
 loop_ 

Saulius Gra\<zulis
2011-03-03

It appeares that the correct formula for this compound is ZrP1.4S0.6
(checked by inspecting atom sites, a formula in the paper title and
the open-access PDF file of the paper). Therefore, the
chemical_formula_moiety and the _chemical_formula_sum values were
corrected as follows:

 _chemical_formula_moiety      'Zr P1.4 S0.6'
 _chemical_formula_sum         'Zr P1.4 S0.6'

Saulius Gra\<zulis
2011-03-04
;
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_original_formula_sum        'Zr P1.4 S0.6'
_cod_database_code               8103035