data_MgBH4_0p56Kr #============================================================================= 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 'B2 H8 Kr0.557, Mg' _chemical_formula_sum 'B2 H8 Kr0.557, Mg' _chemical_formula_weight 100.68 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 15.562(2) _cell_length_b 15.562(2) _cell_length_c 15.562(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3768.8(10) _cell_formula_units_Z 24 _cell_measurement_temperature 115 _cell_special_details ; ? ; # The next five fields are character fields that describe the specimen. _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 ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_crystal_description 'block' #============================================================================= # 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 115 _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 ? # 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 ; 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. ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # 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 0.4380 _pd_proc_ls_prof_wR_factor 0.6381 _pd_proc_ls_prof_wR_expected 0.0599 # 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 17.4638 _pd_proc_ls_prof_cwR_factor 10.0197 _pd_proc_ls_prof_cwR_expected 0.9404 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 113.5114 _pd_proc_ls_prof_echi2 113.5114 # Items related to LS refinement _refine_ls_goodness_of_fit_all 10.6542 _refine_ls_R_I_factor 10.4314 _refine_ls_number_reflns 164 _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) # 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 0.12500 0.12500 0.12500 0.08882 0.836(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 2.3832(2) 1_555 ? Mg H1 1.97363(18) 1_555 ? Mg H2 1.9340(2) 1_555 ? B1 H1 1.20451(11) 1_555 ? B1 H2 1.20509(15) 1_555 ? B1 Kr2 4.9433(4) 1_555 ? B1 Kr2 5.0090(6) 13_555 ? B1 Kr2 4.0671(4) 39_545 ? H1 Kr2 3.9502(3) 4_555 ? H1 Kr2 3.5121(3) 39_545 ? H2 Kr2 4.8653(5) 1_555 ? H2 Kr2 3.9213(5) 13_555 ? H2 Kr2 4.8641(5) 39_545 ? 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 132.56(2) 1_555 20_455 ? H1 Mg H1 69.348(11) 1_555 51_556 ? H1 Mg H1 132.56(2) 1_555 66_555 ? H1 Mg H2 60.463(10) 1_555 1_555 ? H1 Mg H2 90.062(14) 1_555 20_455 ? H1 Mg H2 129.194(18) 1_555 51_556 ? H1 Mg H2 81.950(11) 1_555 66_555 ? H1 Mg H1 132.56(2) 20_455 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 109.47(2) 1_555 88_545 ? H1 B1 H2 109.499(19) 1_555 1_555 ? H1 B1 H2 109.491(16) 1_555 88_545 ? H2 B1 H2 109.379(17) 1_555 88_545 ? # start Validation Reply Form _vrf_PLAT041__MgBH4_0p56Kr ; PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check RESPONSE: Can be due to rounding of Kr0.557 to Kr 0.56 or vice versa ; _vrf_PLAT077__MgBH4_0p56Kr ; PROBLEM: Unitcell Contains Non-integer Number of Atoms .. Please Check RESPONSE: Kr atoms are not fully occupied ; _vrf_PLAT751__MgBH4_0p56Kr ; PROBLEM: Bond Calc 1.97000, Rep 1.97363(18) ...... Senseless s.u. RESPONSE: the coordinates of B and H atoms were not refined ; _vrf_PLAT752__MgBH4_0p56Kr ; PROBLEM: Angle Calc 60.00, Rep 60.46(1) ...... Senseless s.u. RESPONSE: the coordinates of B and H atoms were not refined ; # end Validation Reply Form