data_MgBH4_0p40Kr_phase1
# Definition of non standard CIF items (Reliability indices used in FULLPROF) 
 
loop_ 
_publ_manuscript_incl_extra_item
_publ_manuscript_incl_extra_info
_publ_manuscript_incl_extra_defn
#      Name                               Explanation                 Standard?
#     ------                              -----------                 ---------
 '_pd_proc_ls_prof_cR_factor'    'Prof. R-factor CORRECTED for background'   no
 '_pd_proc_ls_prof_cwR_factor'   'wProf.R-factor CORRECTED for background'   no
 '_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background'   no
 '_pd_proc_ls_prof_chi2'         'Chi-square for all considered points'      no
 '_pd_proc_ls_prof_echi2'        'Chi-2 for points with Bragg contribution'  no
#=============================================================================
# 5. CHEMICAL DATA
 
_chemical_name_systematic
; ?
;
_chemical_name_common             'Magnesium borohydride'
_chemical_formula_moiety          '0.404(Kr), 2(B H4), Mg'
_chemical_formula_sum             'B2 H8 Kr0.40 Mg'
_chemical_formula_weight          87.88
 
loop_
    _atom_type_symbol               
    _atom_type_scat_Cromer_Mann_a1 
    _atom_type_scat_Cromer_Mann_b1 
    _atom_type_scat_Cromer_Mann_a2 
    _atom_type_scat_Cromer_Mann_b2 
    _atom_type_scat_Cromer_Mann_a3 
    _atom_type_scat_Cromer_Mann_b3 
    _atom_type_scat_Cromer_Mann_a4 
    _atom_type_scat_Cromer_Mann_b4 
    _atom_type_scat_Cromer_Mann_c 
    _atom_type_scat_dispersion_real 
    _atom_type_scat_dispersion_imag 
    _atom_type_scat_source          
mg     5.42040   2.82750   2.17350  79.26110   1.22690   0.38080
       2.30730   7.19370   0.85840   0.04200   0.03600
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
b      2.05450  23.21850   1.33260   1.02100   1.09790  60.34980
       0.70680   0.14030  -0.19320   0.00000   0.00100
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
h      0.49300  10.51090   0.32291  26.12570   0.14019   3.14236
       0.04081  57.79970   0.00304   0.00000   0.00000
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
kr    17.35550   1.93840   6.72860  16.56230   5.54930   0.22610
       3.53750  39.39720   2.82500  -0.65200   2.71300
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
 
#=============================================================================
 
# 6. POWDER SPECIMEN AND CRYSTAL DATA
 
_symmetry_cell_setting                Cubic
_symmetry_space_group_name_H-M       'I a -3 d'
_symmetry_space_group_name_Hall      '-I 4bd 2c 3'
 
loop_
    _symmetry_equiv_pos_as_xyz   #<--must include 'x,y,z'
'x,y,z'
'x+1/2,-y+1/2,-z'
'-x,y+1/2,-z+1/2'
'-x+1/2,-y,z+1/2'
'y,z,x'
'-y+1/2,-z,x+1/2'
'y+1/2,-z+1/2,-x'
'-y,z+1/2,-x+1/2'
'z,x,y'
'-z,x+1/2,-y+1/2'
'-z+1/2,-x,y+1/2'
'z+1/2,-x+1/2,-y'
'y+1/4,x+1/4,z+1/4'
'-y+3/4,x+3/4,-z+1/4'
'y+3/4,-x+1/4,-z+3/4'
'-y+1/4,-x+3/4,z+3/4'
'z+1/4,y+1/4,x+1/4'
'-z+1/4,-y+3/4,x+3/4'
'-z+3/4,y+3/4,-x+1/4'
'z+3/4,-y+1/4,-x+3/4'
'x+1/4,z+1/4,y+1/4'
'x+3/4,-z+1/4,-y+3/4'
'-x+1/4,-z+3/4,y+3/4'
'-x+3/4,z+3/4,-y+1/4'
'-x,-y,-z'
'-x+1/2,y+1/2,z'
'x,-y+1/2,z+1/2'
'x+1/2,y,-z+1/2'
'-y,-z,-x'
'y+1/2,z,-x+1/2'
'-y+1/2,z+1/2,x'
'y,-z+1/2,x+1/2'
'-z,-x,-y'
'z,-x+1/2,y+1/2'
'z+1/2,x,-y+1/2'
'-z+1/2,x+1/2,y'
'-y+3/4,-x+3/4,-z+3/4'
'y+1/4,-x+1/4,z+3/4'
'-y+1/4,x+3/4,z+1/4'
'y+3/4,x+1/4,-z+1/4'
'-z+3/4,-y+3/4,-x+3/4'
'z+3/4,y+1/4,-x+1/4'
'z+1/4,-y+1/4,x+3/4'
'-z+1/4,y+3/4,x+1/4'
'-x+3/4,-z+3/4,-y+3/4'
'-x+1/4,z+3/4,y+1/4'
'x+3/4,z+1/4,-y+1/4'
'x+1/4,-z+1/4,y+3/4'
'x+1/2,y+1/2,z+1/2'
'x,-y,-z+1/2'
'-x+1/2,y,-z'
'-x,-y+1/2,z'
'y+1/2,z+1/2,x+1/2'
'-y,-z+1/2,x'
'y,-z,-x+1/2'
'-y+1/2,z,-x'
'z+1/2,x+1/2,y+1/2'
'-z+1/2,x,-y'
'-z,-x+1/2,y'
'z,-x,-y+1/2'
'y+3/4,x+3/4,z+3/4'
'-y+1/4,x+1/4,-z+3/4'
'y+1/4,-x+3/4,-z+1/4'
'-y+3/4,-x+1/4,z+1/4'
'z+3/4,y+3/4,x+3/4'
'-z+3/4,-y+1/4,x+1/4'
'-z+1/4,y+1/4,-x+3/4'
'z+1/4,-y+3/4,-x+1/4'
'x+3/4,z+3/4,y+3/4'
'x+1/4,-z+3/4,-y+1/4'
'-x+3/4,-z+1/4,y+1/4'
'-x+1/4,z+1/4,-y+3/4'
'-x+1/2,-y+1/2,-z+1/2'
'-x,y,z+1/2'
'x+1/2,-y,z'
'x,y+1/2,-z'
'-y+1/2,-z+1/2,-x+1/2'
'y,z+1/2,-x'
'-y,z,x+1/2'
'y+1/2,-z,x'
'-z+1/2,-x+1/2,-y+1/2'
'z+1/2,-x,y'
'z,x+1/2,-y'
'-z,x,y+1/2'
'-y+1/4,-x+1/4,-z+1/4'
'y+3/4,-x+3/4,z+1/4'
'-y+3/4,x+1/4,z+3/4'
'y+1/4,x+3/4,-z+3/4'
'-z+1/4,-y+1/4,-x+1/4'
'z+1/4,y+3/4,-x+3/4'
'z+3/4,-y+3/4,x+1/4'
'-z+3/4,y+1/4,x+3/4'
'-x+1/4,-z+1/4,-y+1/4'
'-x+3/4,z+1/4,y+3/4'
'x+1/4,z+3/4,-y+3/4'
'x+3/4,-z+3/4,y+1/4'
 
_cell_length_a                       15.7621(2)
_cell_length_b                       15.7621(2)
_cell_length_c                       15.7621(2)
_cell_angle_alpha                    90.0000
_cell_angle_beta                     90.0000
_cell_angle_gamma                    90.0000
_cell_volume                         3915.98(11)
_cell_formula_units_Z                24
_cell_measurement_temperature        200
_cell_special_details
; ?
;
# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.
 
_pd_spec_mount_mode               'transmission'       # options are 'reflection'
                                          # or 'transmission'
_pd_spec_shape                    'cylinder'       # options are 'cylinder' 
                                          # 'flat_sheet' or 'irregular'
_pd_char_colour                   'white'       # use ICDD colour descriptions
 
# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was 
# prepared is in kPa.  The temperature of preparation is in K.        
 
_pd_prep_cool_rate                6
_pd_prep_pressure                 ?
_pd_prep_temperature              ?
 
# The next four fields are normally only needed for transmission experiments.
 
_exptl_crystal_description           'block'
_exptl_absorpt_coefficient_mu        ?
_exptl_absorpt_correction_type       'none'
_exptl_absorpt_process_details       ?
_exptl_absorpt_correction_T_min      ?
_exptl_absorpt_correction_T_max      ?
 
#=============================================================================
 
# 7. EXPERIMENTAL DATA
 
_exptl_special_details
; ?
;
 
# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.
 
_pd_instr_location
; BM01 at the ESRF
;
_pd_calibration_special_details           # description of the method used
                                          # to calibrate the instrument
; LaB6 callibrant for area detctor
;
 
_diffrn_ambient_temperature          200
_diffrn_source             'synchrotron' 
_diffrn_radiation_type     'synchrotron' 
_diffrn_radiation_wavelength       0.67522
 
_diffrn_radiation_monochromator      'Si'
_diffrn_measurement_device_type      'pixel area detector'
_diffrn_measurement_method           ?
_diffrn_detector_area_resol_mean     5.81 
_diffrn_detector                     'Pilatus 2M'
_diffrn_detector_type                'Pilatus@SNBL' # make or model of detector
_pd_meas_scan_method      'fixed'   # options are 'step', 'cont',
                              # 'tof', 'fixed' or
                              # 'disp' (= dispersive)
_pd_meas_special_details
;  ?
;
 
#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.
 
_pd_meas_number_of_points         3352
_pd_meas_2theta_range_min         0.06783
_pd_meas_2theta_range_max         35.03902
_pd_meas_2theta_range_inc         0.010439
 
#=============================================================================
 
# 8. REFINEMENT DATA
 
_refine_special_details
; ?
;
 
# Use the next field to give any special details about the fitting of the
# powder pattern.
 
_pd_proc_ls_special_details
; The coordinates of Mg B H atoms were fixed for 2 phases.
Biso was fixed as 2.78 for Mg, 2.87 for B, 
4.87 for H and 8.82 for Kr.
In order avoid the corelation between Kr occupanices 
and thermal dissplacment parameters, Boverall was 
refined with fixed Biso, as mentioned before.
;
 
# The next three items are given as text.
 
_pd_proc_ls_profile_function      'pseudo-Voigt'
_pd_proc_ls_background_function   'manual'
_pd_proc_ls_pref_orient_corr
; ?
;
 
#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard
 
_pd_proc_ls_prof_R_factor                0.3918
_pd_proc_ls_prof_wR_factor               0.5676
_pd_proc_ls_prof_wR_expected             0.0687
 
#  The following profile R-factors are CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These items are not in the current CIF standard, but are defined above
 
_pd_proc_ls_prof_cR_factor               16.6261
_pd_proc_ls_prof_cwR_factor               9.0941
_pd_proc_ls_prof_cwR_expected             1.1011
 
#  The following items are not in the CIF standard, but are defined above
 
_pd_proc_ls_prof_chi2                68.2170
_pd_proc_ls_prof_echi2               68.2170
 
#  Items related to LS refinement
 
_refine_ls_R_I_factor                 7.5697
_refine_ls_goodness_of_fit_all       8.2594  
_refine_ls_number_reflns                   163
_refine_ls_number_parameters                31
_refine_ls_number_restraints                 0
_refine_ls_shift/su_max                   0.01
 
# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
 
_pd_proc_2theta_range_min                0.0588
_pd_proc_2theta_range_max               35.0300
_pd_proc_2theta_range_inc              0.010439
_pd_proc_wavelength                    0.675220
 
_pd_block_diffractogram_id        ?  # The id used for the block containing
                                     # the powder pattern profile (section 11)
 
# Give appropriate details in the next two text fields.
 
_pd_proc_info_excluded_regions    ?
_pd_proc_info_data_reduction      ?
 
# The following items are used to identify the programs used.
 
_computing_data_collection           PILATUS@SNBL
_computing_structure_solution        FOX
_computing_structure_refinement      FULLPROF
_computing_molecular_graphics        ?
_computing_publication_material      ?
 
#=============================================================================
 
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
 
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_occupancy
    _atom_site_adp_type
    _atom_site_type_symbol
 Mg  0.25000  0.12500  0.50000  0.01915  1.00000 Uiso Mg    
 B1  0.30980  0.05980  0.37500  0.02512  1.00000 Uiso B     
 H1  0.28570  0.02070  0.43730  0.05045  1.00000 Uiso H     
 H2  0.29740  0.13550  0.38560  0.05045  1.00000 Uiso H     
 Kr2  0.10664  0.10664  0.10664  0.08882  0.3033(18) Uiso Kr    
 
# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.
 
#=============================================================================
 
# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY 
 
_geom_special_details                ?
 
loop_
   _geom_bond_atom_site_label_1
   _geom_bond_atom_site_label_2
   _geom_bond_distance
   _geom_bond_site_symmetry_2
   _geom_bond_publ_flag         
Mg    B1    2.41382(2)    1_555 ?
Mg    H1    1.99901(2)    1_555 ?
Mg    H2    1.95884(2)    1_555 ?
B1    H1    1.22000(1)   1_555 ?
B1    H2    1.22058(2)   1_555 ?
B1    Kr2   4.14976(4)   39_545 ?
B1    Kr2   4.68486(4)   85_555 ?
B1    Kr2   5.35645(5)   88_545 ?
H1    Kr2   3.65199(3)   39_545 ?
H1    Kr2   3.53186(3)   50_555 ?
H2    Kr2   4.33845(5)   73_555 ?
H2    Kr2   3.63729(4)   13_555 ?
H2    Kr2   4.52650(4)   85_555 ?

loop_
   _geom_angle_atom_site_label_1
   _geom_angle_atom_site_label_2
   _geom_angle_atom_site_label_3
   _geom_angle
   _geom_angle_site_symmetry_1
   _geom_angle_site_symmetry_3
   _geom_angle_publ_flag
 H1   Mg   H1    132.559(2)     1_555   20_455 ?
 H1   Mg   H1    69.3483(11)    1_555   51_556 ?
 H1   Mg   H1    132.56(2)      1_555   66_555 ?
 H1   Mg   H2    60.4633(10)    1_555    1_555 ?
 H1   Mg   H2    90.0616(14)    1_555   20_455 ?
 H1   Mg   H2    129.194(2)     1_555   51_556 ?
 H2   Mg   H2    90.409(16)     1_555   20_455 ?
 H2   Mg   H2    170.31(3)      1_555   51_556 ?
 H2   Mg   H2    90.409(16)     1_555   66_555 ?
 H2   Mg   H2    90.409(16)    20_455   51_556 ?
 H1   B1   H1    109.468(2)     1_555   88_545 ?
 H1   B1   H2    109.499(2)    1_555    1_555 ?
 H1   B1   H2    109.491(2)    1_555   88_545 ?
 H1   B1   H2    109.491(2)    88_545    1_555 ?
 H2   B1   H2    109.379(2)    1_555   88_545 ?
# start Validation Reply Form
_vrf_PLAT077_MgBH4_0p40Kr_phase1
;
PROBLEM: Unitcell Contains Non-integer Number of Atoms ..     Please Check 
RESPONSE: Kr atom sites are not fully occupied
;
_vrf_PLAT751_MgBH4_0p40Kr_phase1
;
PROBLEM: Bond    Calc     2.00000, Rep  1.99901(2) ......  Senseless s.u.  
RESPONSE: the coordinates of B and H atoms were not refined
the calculations are based on unit cell parameters refinement only.
;
_vrf_PLAT752_MgBH4_0p40Kr_phase1
;
PROBLEM: Angle   Calc       60.00, Rep       60.46 ......  Senseless s.u.  
RESPONSE: the coordinates of B and H atoms were not refined
the calculations are based on unit cell parameters refinement only.
;
# end Validation Reply Form