 
#=============================================================================
 data_global
#=============================================================================
 
 
_journal_name_full                   'Dalton Trans.'
 
#=============================================================================
 
#  SUBMISSION DETAILS
 
_publ_contact_author_name            'B. Marler'
_publ_contact_author_address            
;     
Dept. of Geology, Mineralogy and Geophysics, Ruhr University Bochum, 
D-44780 Bochum, Germany ; Tel: (+49) 234-32-23514
;
_publ_contact_author_email           bernd.marler@rub.de
_publ_contact_author_fax             ?
_publ_contact_author_phone           '(+49) 234-32-23514'
 
_publ_requested_journal              'Dalton Trans.'
 
#=============================================================================
 
# 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
#=============================================================================
 
#  TITLE AND AUTHOR LIST
 
_publ_section_title
; 
TOPOTACTIC CONDENSATION OF LAYER SILICATES WITH FERRIERITE-TYPE LAYERS FORMING 
POROUS TECTOSILICATES
;
_publ_section_title_footnote
;
;
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary.
 
loop_
    _publ_author_name
    _publ_author_address
'Marler, B.'
; 
Dept. of Geology, Mineralogy and Geophysics, Ruhr University Bochum, 
D-44780 Bochum, Germany
;
'Wang, Y.'
; 
College of Chemistry and Molecular Engineering, Peking University, 
Beijing 100871,China
;
'Song, J.'
;
Beijing University of Chemical Technology, State Key Lab of Chemical 
Resource Engineering, Beijing 100029, China
;
'Gies, H.'
; 
Dept. of Geology, Mineralogy and Geophysics, Ruhr University Bochum, 
D-44780 Bochum, Germany
;
#=============================================================================
 
#  TEXT
 

_publ_section_abstract
; 
see article
;          

#=============================================================================

#  CHEMICAL DATA
 
_chemical_name_systematic
; ?
;
_chemical_name_common             'RUB-48'
_chemical_formula_moiety          'C28 H76 N4 O76 Si36'
_chemical_formula_structural      ?
_chemical_formula_analytical      [Si36O72(OH)4](C7H18N)4
_chemical_formula_iupac           ?
_chemical_formula_sum             'C28 H76 N4 O76 Si36'
_chemical_formula_weight          2696.0
_chemical_melting_point           ?
_chemical_compound_source         ?       
 
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          
si     6.29150   2.43860   3.03530  32.33370   1.98910   0.67850
       1.54100  81.69370   1.14070   0.24400   0.33000
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o      3.04850  13.27710   2.28680   5.70110   1.54630   0.32390
       0.86700  32.90890   0.25080   0.04700   0.03200
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c      2.31000  20.84390   1.02000  10.20750   1.58860   0.56870
       0.86500  51.65120   0.21560   0.01700   0.00900
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n     12.21260   0.00570   3.13220   9.89330   2.01250  28.99750
       1.16630   0.58260 -11.52900   0.02900   0.01800
 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
 
#=============================================================================
 
#  POWDER SPECIMEN AND CRYSTAL DATA
 
_symmetry_cell_setting                Orthorhombic
_symmetry_space_group_name_H-M       'C m c m'
_symmetry_space_group_name_Hall      '-C 2c 2'
 
loop_
    _symmetry_equiv_pos_as_xyz   #<--must include 'x,y,z'
'x,y,z'
'x,-y,-z'
'-x,y,-z+1/2'
'-x,-y,z+1/2'
'-x,-y,-z'
'-x,y,z'
'x,-y,z+1/2'
'x,y,-z+1/2'
'x+1/2,y+1/2,z'
'x+1/2,-y+1/2,-z'
'-x+1/2,y+1/2,-z+1/2'
'-x+1/2,-y+1/2,z+1/2'
'-x+1/2,-y+1/2,-z'
'-x+1/2,y+1/2,z'
'x+1/2,-y+1/2,z+1/2'
'x+1/2,y+1/2,-z+1/2'
 
_cell_length_a                       7.369(1)
_cell_length_b                       22.559(3)
_cell_length_c                       13.993(2)
_cell_angle_alpha                    90.00000
_cell_angle_beta                     90.00000
_cell_angle_gamma                    90.00000
_cell_volume                         2326.2(4)
_cell_formula_units_Z                1
_cell_measurement_temperature        298
_cell_special_details
; ?
;

 
# The next five fields are character fields that describe the specimen.
 
_pd_spec_mounting                         
;                               glass capillary
;
_pd_spec_mount_mode               'transmission'
_pd_spec_shape                    'cylinder'
_pd_char_particle_morphology      'plates'
_pd_char_colour                   white
 
 
# 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_density_meas          ?
_exptl_crystal_density_diffrn        1.925
_exptl_crystal_density_method       'not measured'
 
#=============================================================================
 
#  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
; ?
;
_pd_calibration_special_details           # description of the method used
                                          # to calibrate the instrument
; ?
;
 
_diffrn_ambient_temperature          298(2)
_diffrn_source                       'X-ray tube'
_diffrn_radiation_type               'Cu K\a1' 
_diffrn_source_target                Cu
 
_diffrn_radiation_monochromator      'Ge(111)'
_diffrn_measurement_device_type      'Siemens D5000'
_diffrn_measurement_method           ?
_diffrn_detector_area_resol_mean     ?   # Not in version 2.0.1
_diffrn_detector                     ?
_diffrn_detector_type                'Braun PSD'
_pd_meas_scan_method                 'step'
_pd_meas_special_details
;  ?
;
 
_diffrn_radiation_wavelength        1.5406

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.
 
_pd_meas_number_of_points         11837
_pd_meas_2theta_range_min         3.04700
_pd_meas_2theta_range_max         94.98900
_pd_meas_2theta_range_inc         0.007768
 
#=============================================================================
 
#  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 next three items are given as text.
 
_pd_proc_ls_profile_function      'pseudo-Voigt'
_pd_proc_ls_background_function   'background points'
_pd_proc_ls_pref_orient_corr
;                                 'none'
;
 
 
#  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                1.9540
_pd_proc_ls_prof_wR_factor               2.6671
_pd_proc_ls_prof_wR_expected             2.3640
 
#  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               26.4202
_pd_proc_ls_prof_cwR_factor              18.2707
_pd_proc_ls_prof_cwR_expected            16.1942
 
#  The following items are not in the CIF standard, but are defined above
 
_pd_proc_ls_prof_chi2                 1.2729
_pd_proc_ls_prof_echi2                1.2729
 
#  Items related to LS refinement
 
_refine_ls_R_I_factor                 5.4923
_refine_ls_number_reflns                   686
_refine_ls_number_parameters                37
_refine_ls_number_restraints                45
_refine_ls_goodness_of_fit_all             1.13
_refine_ls_shift/su_max                    0.02
_refine_ls_hydrogen_treatment             none  

 
# 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                3.0262
_pd_proc_2theta_range_max               94.9682
_pd_proc_2theta_range_inc              0.007768
_pd_proc_wavelength                    1.540600
 
_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    0
_pd_proc_info_data_reduction      ?
 
# The following items are used to identify the programs used.
 
_computing_data_collection           ?
_computing_structure_solution        ?
_computing_structure_refinement      FULLPROF
_computing_molecular_graphics        ?
_computing_publication_material      ?
 
#=============================================================================
 
#  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              # Not in version 2.0.1
    _atom_site_type_symbol
 Si1   0.2093(7)   0.2290(3)   0.25000     0.0148(7)   1.00000    Uiso Si  
 Si2   0.2955(5)   0.1888(2)   0.0459(3)   0.0148(7)   1.00000    Uiso Si  
 Si3   0.00000     0.1113(3)   0.5480(4)   0.0148(7)   1.00000    Uiso Si  
 Si4   0.00000     0.1735(4)   0.75000     0.0148(7)   1.00000    Uiso Si  
 O1   0.2503(11)  0.1923(4)   0.1573(4)   0.0222(17)  1.00000    Uiso O   
 O2   0.00000     0.2453(7)   0.25000     0.0222(17)  1.00000    Uiso O   
 O3   0.3157(11)  0.2901(4)   0.25000     0.0222(17)  1.00000    Uiso O   
 O4   0.1778(10)  0.1387(4)  -0.0015(7)   0.0222(17)  1.00000    Uiso O   
 O5   0.50000     0.1719(6)   0.0282(9)   0.0222(17)  1.00000    Uiso O   
 O6   0.25000     0.25000     0.00000     0.0222(17)  1.00000    Uiso O   
 O7   0.00000     0.1331(5)   0.6572(6)   0.0222(17)  1.00000    Uiso O   
 O8   0.50000     0.4587(3)   0.4492(9)   0.0222(17)  1.00000    Uiso O   
 C1   0.50000    -0.0833(9)   0.25000     0.300(16)   1.50000    Uiso C   
 N1   0.50000    -0.0173(10)  0.25000     0.300(16)   1.00000    Uiso N   
 C2   0.398(2)    0.0295(9)   0.1982(15)  0.300(16)   0.811(12)  Uiso C   
 C4   0.50000     0.0007(17)  0.0985(16)  0.300(16)   0.81(2)    Uiso C   
 C3   0.193(3)    0.035(2)    0.25000     0.300(16)   0.81(2)    Uiso C   
 
# The occupancy factor of the carbon atom C1 was adjusted to account also 
# for the scattering power of the hydrogen atoms bonded to C1 (CH3-group).  
# The positions of C2, C3 and C4 do not represent the correct geometry of 
# the dynamically disordered organic cation.  
#=============================================================================
 
#  DISTANCES AND ANGLES / MOLECULAR GEOMETRY 
 
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
Si1   Si1   3.085(7)      3_555 ?
Si1   Si2   3.063(5)          . ?
Si1   Si2   3.063(5)      8_555 ?
Si1   Si4   3.070(9)     10_556 ?
Si1   O1    1.568(8)          . ?
Si1   O1    1.568(8)      8_555 ?
Si1   O2    1.586(6)          . ?
Si1   O3    1.586(11)         . ?
Si2   Si1   3.063(5)          . ?
Si2   Si2   3.014(5)      6_655 ?
Si2   Si2   3.118(6)     13_555 ?
Si2   Si3   3.086(6)      3_555 ?
Si2   O1    1.596(7)          . ?
Si2   O4    1.571(10)         . ?
Si2   O5    1.574(5)          . ?
Si2   O6    1.559(4)          . ?
Si3   Si2   3.086(6)      3_555 ?
Si3   Si2   3.086(6)      8_555 ?
Si3   Si4   3.156(7)          . ?
Si3   O4    1.588(9)      3_555 ?
Si3   O4    1.588(9)      8_555 ?
Si3   O7    1.605(10)         . ?
Si3   O8    1.580(10)    10_456 ?
Si4   Si1   3.070(9)     10_456 ?
Si4   Si1   3.070(9)     12_555 ?
Si4   Si3   3.156(7)          . ?
Si4   Si3   3.156(7)      3_556 ?
Si4   O3    1.587(10)    10_456 ?
Si4   O3    1.587(10)    12_555 ?
Si4   O7    1.586(11)         . ?
Si4   O7    1.586(11)     3_556 ?
O1    Si1   1.568(8)          . ?
O1    Si2   1.596(7)          . ?
O1    O1    2.594(8)      8_555 ?
O1    O2    2.552(11)         . ?
O1    O3    2.604(11)         . ?
O1    O4    2.586(12)         . ?
O1    O5    2.619(11)         . ?
O1    O6    2.557(7)          . ?
O2    Si1   1.586(6)          . ?
O2    Si1   1.586(6)      3_555 ?
O2    O1    2.552(11)         . ?
O2    O1    2.552(11)     3_555 ?
O2    O1    2.552(11)     6_555 ?
O2    O1    2.552(11)     8_555 ?
O2    O3    2.537(10)         . ?
O2    O3    2.537(10)     3_555 ?
O3    Si1   1.586(11)         . ?
O3    Si4   1.587(10)    10_556 ?
O3    O1    2.604(11)         . ?
O3    O1    2.604(11)     8_555 ?
O3    O2    2.537(10)         . ?
O3    O3    2.716(11)     3_655 ?
O3    O7    2.556(12)    10_556 ?
O3    O7    2.556(12)    12_554 ?
O4    Si2   1.571(10)         . ?
O4    Si3   1.588(9)      3_555 ?
O4    O1    2.586(12)         . ?
O4    O4    2.621(10)     6_555 ?
O4    O5    2.524(9)          . ?
O4    O6    2.567(9)          . ?
O4    O7    2.545(12)     3_555 ?
O4    O8    2.650(11)    12_554 ?
O5    Si2   1.574(5)          . ?
O5    Si2   1.574(5)      6_655 ?
O5    O1    2.619(11)         . ?
O5    O1    2.619(11)     6_655 ?
O5    O4    2.524(9)          . ?
O5    O4    2.524(9)      6_655 ?
O5    O6    2.580(9)          . ?
O5    O6    2.580(9)      6_655 ?
O6    Si2   1.559(4)          . ?
O6    Si2   1.559(4)     13_555 ?
O6    O1    2.557(7)          . ?
O6    O1    2.557(7)     13_555 ?
O6    O4    2.567(9)          . ?
O6    O4    2.567(9)     13_555 ?
O6    O5    2.580(9)          . ?
O6    O5    2.580(9)     10_455 ?
O7    Si3   1.605(10)         . ?
O7    Si4   1.586(11)         . ?
O7    O3    2.556(12)    10_456 ?
O7    O3    2.556(12)    12_555 ?
O7    O4    2.545(12)     3_555 ?
O7    O4    2.545(12)     8_555 ?
O7    O7    2.597(12)     3_556 ?
O7    O8    2.551(14)    10_456 ?
O8    Si3   1.580(10)    10_556 ?
O8    O4    2.650(11)    12_555 ?
O8    O4    2.650(11)    15_555 ?
O8    O7    2.551(14)    10_556 ?
O8    O8    2.344(13)     2_566 ?
C1    N1    1.49(3)           . ?
C1    C2    2.75(3)           . ?
C1    C2    2.75(3)       3_655 ?
C1    C2    2.75(3)       6_655 ?
C1    C2    2.75(3)       8_555 ?
C1    C4    2.84(3)           . ?
C1    C4    2.84(3)       3_655 ?
N1    C1    1.49(3)           . ?
N1    C2    1.48(3)           . ?
N1    C2    1.48(3)       3_655 ?
N1    C2    1.48(3)       6_655 ?
N1    C2    1.48(3)       8_555 ?
N1    C4    2.16(2)           . ?
N1    C4    2.16(2)       3_655 ?
N1    C3    2.55(3)           . ?
N1    C3    2.55(3)       3_655 ?
C2    C1    2.75(3)           . ?
C2    N1    1.48(3)           . ?
C2    C2    2.09(3)       3_655 ?
C2    C2    1.50(2)       6_655 ?
C2    C2    1.45(3)       8_555 ?
C2    C4    1.71(3)           . ?
C2    C4    3.01(3)       3_655 ?
C2    C3    1.68(3)           . ?
C2    C3    3.10(3)       3_655 ?
C4    C1    2.84(3)           . ?
C4    N1    2.16(2)           . ?
C4    C2    1.71(3)           . ?
C4    C2    3.01(3)       3_655 ?
C4    C2    1.71(3)       6_655 ?
C4    C2    3.01(3)       8_555 ?
C4    C4    2.76(3)       2_555 ?
C4    C3    3.20(3)           . ?
C4    C3    3.20(3)       3_655 ?
C3    N1    2.55(3)           . ?
C3    C2    1.68(3)           . ?
C3    C2    3.10(3)       3_655 ?
C3    C2    3.10(3)       6_655 ?
C3    C2    1.68(3)       8_555 ?
C3    C4    3.20(3)           . ?
C3    C4    3.20(3)       3_655 ?
C3    C3    2.84(3)       3_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
 O1   Si1  O1   111.6(6)       5_555    6_556 ?
 O1   Si1  O2   108.1(7)       5_555    7_555 ?
 O1   Si1  O3   111.3(8)       5_555    8_555 ?
 O1   Si1  O2   108.1(7)       6_556    7_555 ?
 O1   Si1  O3   111.3(8)       6_556    8_555 ?
 O2   Si1  O3   106.2(8)       7_555    8_555 ?
 O1   Si2  O4   109.4(8)       5_555    6_555 ?
 O1   Si2  O5   111.4(8)       5_555    7_555 ?
 O1   Si2  O6   108.3(5)       5_555    8_555 ?
 O4   Si2  O5   106.7(7)       6_555    7_555 ?
 O4   Si2  O6   110.1(7)       6_555    8_555 ?
 O5   Si2  O6   110.8(6)       7_555    8_555 ?
 O4   Si3  O4   111.2(8)       4_556    5_556 ?
 O4   Si3  O7   105.7(8)       4_556    6_555 ?
 O4   Si3  O8   113.5(8)       4_556    7_566 ?
 O4   Si3  O7   105.7(8)       5_556    6_555 ?
 O4   Si3  O8   113.5(8)       5_556    7_566 ?
 O7   Si3  O8   106.4(9)       6_555    7_566 ?
 O3   Si4  O3   117.7(9)       5_566    6_666 ?
 O3   Si4  O7   107.3(8)       5_566    7_555 ?
 O3   Si4  O7   107.3(8)       5_566    8_557 ?
 O3   Si4  O7   107.3(8)       6_666    7_555 ?
 O3   Si4  O7   107.3(8)       6_666    8_557 ?
 O7   Si4  O7   109.9(9)       7_555    8_557 ?
