Crystal structure of the high-pressure phase of the oxonitridosilicate chloride Ce~4~[Si~4~O~3+<i>x~</i>N~7{-~<i>x</i>}]Cl~1{-~<i>x</i>}O~<i>x~</i>, <i>x</i> ≃0.2
Friedrich, Alexandra; Haussuehl, Eiken; Morgenroth, Wolfgang; Lieb, Alexandra; Winkler, Björn; Knorr, Karsten; Schnick, Wolfgang; Acta Crystallographica Section B 62 (2006) 205–211; doi:10.1107/S0108768106003302

data_2100407
_publ_section_title
;
 Crystal structure of the high-pressure phase of the oxonitridosilicate
 chloride
 Ce~4~[Si~4~O~3+<i>x~</i>N~7{-~<i>x</i>}]Cl~1{-~<i>x</i>}O~<i>x~</i>,
 <i>x</i> \\simeq 0.2
;
_journal_coeditor_code           BK5022
_journal_date_accepted           2006-01-26
_journal_date_recd_electronic    2005-09-10
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              205
_journal_page_last               211
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768106003302
_journal_volume                  62
_journal_year                    2006
_chemical_formula_structural     Ce4[Si4O3.07N6.93]Cl0.93O0.07
_chemical_formula_sum            'Ce4 Cl0.92 N6.92 O3.16 Si4'
_chemical_formula_weight         853.05
_chemical_name_systematic
;
cerium oxonitridosilicate chloride
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00(4)
_cell_angle_beta                 90.00(4)
_cell_angle_gamma                90.00(4)
_cell_formula_units_Z            4
_cell_length_a                   10.347(4)
_cell_length_b                   10.347(4)
_cell_length_c                   10.347(4)
_cell_measurement_pressure       '3.0 GPa'
_cell_measurement_reflns_used    10
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.85
_cell_measurement_theta_min      3.7
_cell_volume                     1107.8(7)
_computing_cell_refinement       'DIF4 (Eichhorn, 1987a)'
_computing_data_collection       'DIF4 (Eichhorn, 1987a)'
_computing_data_reduction
'REDUCE (Eichhorn, 1987b); AVSORT (Eichhorn, 1978); ABSORB v6.0 (Angel, 2004)'
_computing_molecular_graphics    'ATOMS (Dowty, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'NaJ point detector'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'HUBER diffractometer D3, HASYLAB/DESY'
_diffrn_measurement_method       'omega scan, continuous, fixed-phi method'
_diffrn_radiation_monochromator  'Si(111) double crystal'
_diffrn_radiation_source         'synchrotron HASYLAB/DESY'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.45000
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1712
_diffrn_reflns_theta_full        13.96
_diffrn_reflns_theta_max         13.96
_diffrn_reflns_theta_min         1.76
_diffrn_standards_interval_time  '50 min'
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    4.482
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x 16 x 16 points =  4096 total grid points
  Based upon method of Burnham (1966)
 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are:
         range of dac transmission factors (min-max)      0.469     0.597
 thickness of diamond anvil 1:  1.300 mm, mu =  0.0958 mm-1
       thickness of platten 1:  4.000 mm, mu =  0.0334 mm-1
 thickness of diamond anvil 2:  1.300 mm, mu =  0.0958 mm-1
       thickness of platten 2:  4.000 mm, mu =  0.0334 mm-1
    No gasket shadowing corrections were made
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
platelike,
 crystal was described in terms of coordinates of corners
 on the orthogonal phi-axis coordinate system of  Busing and Levy (1967)
 (ie +Y along beam, +Z up at circles zero, +X to make right-handed set)
 with origin at the centre of the face of the incident-beam anvil
  loop is over x, y, z (mm)
   0.082426    0.000000    0.127750
   0.092000    0.040000    0.119000
   0.071655    0.000000    0.132699
   0.090000    0.000000    0.102000
   0.098116    0.037494    0.096715
   0.085334    0.000000    0.056894
   0.093706    0.034644    0.060450
   0.096619    0.038697    0.079564
   0.048000    0.000000    0.014000
   0.055975    0.039065    0.016326
  -0.010984    0.000000   -0.003204
  -0.006257    0.017214   -0.001825
   0.045901    0.042720    0.013388
  -0.023931    0.000000    0.018882
  -0.015251    0.024601    0.017570
   0.006709    0.000000    0.144507
   0.037000    0.060000    0.124000
   0.012334    0.060000    0.077570
   0.052282    0.060000    0.121222
   0.054000    0.060000    0.088000
   0.032569    0.060000    0.053963
   0.010000    0.060000    0.068000
   0.019084    0.042390    0.131660
;
_exptl_crystal_F_000             1510
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.864
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(12)
_refine_ls_extinction_coef       0.0067(8)
_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   1.018
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         476
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+16.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                471
_reflns_number_total             476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5022.cif
_cod_data_source_block           3.0GPa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)3
_cod_database_code               2100407
_cod_database_fobs_code          2100407