# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Tomislav Friscic'
_publ_contact_author_email       TF253@CAM.AC.UK
loop_
_publ_author_name
T.Friscic
L.Fabian

data_1
_database_code_depnum_ccdc_archive 'CCDC 707188'

_pd_block_id                     
2008-10-03T15:36|ANHYDR2|Laszlo_Fabian|Philips_Xpert_Pro

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2008-10-03T15:36
_audit_author_name               'Laszlo Fabian'
_audit_update_record             
; 2008-10-03T15:36 Initial CIF as created by GSAS2CIF
;

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
;
Common isotropic displacement parameters were used for all heavy atoms
of the fumarate ion. The Uiso values of H atoms were constrained to be
twice the Uiso values of the heavy atoms they are bonded to.
Bond length and bond angle restraints were based on average values taken
from similar structures in the CSD. Planar group restraints were applied
for the ehtenylene and the carboxylate groups.
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/\s(Y~obs~)^2^
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    1

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
# Rietveld study, this information should be moved into the phase
# blocks)

# The following three fields describe the preparation of the material.
# 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               0
_pd_prep_pressure                100
_pd_prep_temperature             298

_pd_char_colour                  white # use ICDD colour descriptions
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     35
_refine_ls_goodness_of_fit_all   1.03
_refine_ls_number_restraints     15
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
;
zinc fumarate
;
_chemical_name_common            'zinc fumarate'
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  '-C 2yc'

_exptl_crystal_F_000             352
_exptl_crystal_density_diffrn    2.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    DASH

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

# 8. Phase information from GSAS

_pd_phase_name                   Zn-fumarate
_cell_length_a                   8.2406(4)
_cell_length_b                   5.21314(24)
_cell_length_c                   11.4415(6)
_cell_angle_alpha                90.0
_cell_angle_beta                 103.9094(24)
_cell_angle_gamma                90.0
_cell_volume                     477.11(5)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z+1/2
-1 -x,-y,-z
-2 +x,-y,+z+1/2
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z+1/2

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Zn Zn1 0.5 0.15108(25) 0.75 1.0 Uiso 0.0539 4
O O2 0.84422(32) 0.4405(5) 0.80859(21) 1.0 Uiso 0.03512 8
O O3 0.61870(30) 0.3790(5) 0.87699(21) 1.0 Uiso 0.03512 8
C C4 0.75126(32) 0.49685(19) 0.87666(8) 1.0 Uiso 0.03512 8
C C5 0.79427(11) 0.71211(19) 0.96377(7) 1.0 Uiso 0.03512 8
H H6 0.89564(22) 0.7982(5) 0.96430(28) 1.0 Uiso 0.07024 8

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C4 H2 O4 Zn'
_chemical_formula_weight         179.44
_cell_formula_units_Z            4

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O2 1.9277(23) . 101_445 N
Zn1 O3 1.9485(26) . 1_555 N
O2 C4 1.2516(10) . 1_555 N
O3 C4 1.2540(10) . 1_555 N
C4 C5 1.4861(5) . 1_555 N
C5 C5 1.2909(6) . -101_557 N
C5 H6 0.9470(5) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O2 110.58(16) 101_445 . 102_646 N
O2 Zn1 O3 110.17(11) 101_445 . 1_555 N
O2 Zn1 O3 110.47(10) 101_445 . 2_656 N
O3 Zn1 O3 104.84(14) 1_555 . 2_656 N
Zn1 O2 C4 129.88(22) 101_555 . 1_555 N
Zn1 O3 C4 125.31(16) 1_555 . 1_555 N
O2 C4 O3 123.42(19) 1_555 . 1_555 N
O2 C4 C5 120.77(22) 1_555 . 1_555 N
O3 C4 C5 115.81(17) 1_555 . 1_555 N
C4 C5 C5 125.54(5) 1_555 . -101_667 N
C4 C5 H6 115.46(6) 1_555 . 1_555 N
C5 C5 H6 119.00(6) -101_667 . 1_555 N

# Powder diffraction data for histogram 1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
;
Data below 2theta = 8.0 deg. was excluded because of the strongly curved
background in this region. No peaks were apparent in the excluded region.
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# 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
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_measurement_device_type  'Philips Xpert Pro'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder'
# 'flat_sheet' or 'irregular'

loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Zn 4.0 0.000 0.000 14.0743 3.26550 7.03180 0.23330 5.16520 10.3163 2.41000
58.7097 1.30410 International_Tables_Vol_C
O 16.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
C 16.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
H 8.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.539
_diffrn_radiation_wavelength     1.5406
_diffrn_radiation_type           'Cu K\a~1~'
_pd_proc_ls_prof_R_factor        0.0435
_pd_proc_ls_prof_wR_factor       0.0567
_pd_proc_ls_prof_wR_expected     0.0557
_refine_ls_R_Fsqd_factor         0.03578

_pd_proc_ls_background_function  
; GSAS Background function number 1 with 10 terms.
Shifted Chebyshev function of 1st kind
1: 233.103 2: -199.327 3: 91.8388 4: -28.6121
5: 10.8558 6: -1.97561 7: -1.29722 8: 8.03624
9: -7.05808 10: -1.99617
;

_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 3
Surface roughness abs. correction (Suortti)
Terms = 0.28824 0.37815
Correction is refined.
;
_exptl_absorpt_correction_T_min  0.43154
_exptl_absorpt_correction_T_max  0.82796
# Extinction correction
_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000
_pd_proc_ls_pref_orient_corr     
; March-Dollase
AXIS 1 Ratio= 1.15314 h= 1.000 k= 1.000 l= 2.000
Prefered orientation correction range: Min= 0.80878, Max= 1.23595
;

_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 193.316 #2(GV) = 0.000 #3(GW) = 32.143
#4(GP) = 20.004 #5(LX) = 3.386 #6(LY) = 65.899
#7(S/L) = 0.0156 #8(H/L) = 0.0059
#9(trns) = 0.00 #10(shft)= -6.1242
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0020 times the peak
;
_pd_proc_ls_peak_cutoff          0.00200
_pd_proc_info_datetime           2008-10-03T15:36:30
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        4.00419
_pd_meas_2theta_range_max        59.98606
_pd_meas_2theta_range_inc        0.00837
_pd_proc_2theta_range_min        4.00408
_pd_proc_2theta_range_max        59.98596
_pd_proc_2theta_range_inc        0.00837

_pd_meas_number_of_points        6687
_pd_proc_number_of_points        6687

_reflns_number_total             69
_reflns_limit_h_min              0
_reflns_limit_h_max              5
_reflns_limit_k_min              0
_reflns_limit_k_max              3
_reflns_limit_l_min              -8
_reflns_limit_l_max              7
_reflns_d_resolution_high        1.544
_reflns_d_resolution_low         5.553

data_1.2H2O
_database_code_depnum_ccdc_archive 'CCDC 707189'

_pd_block_id                     
2008-09-12T17:39|DIHYDRATE|Laszlo_Fabian|Philips_Xpert_Pro

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2008-09-12T17:39
_audit_author_name               'Laszlo Fabian'
_audit_update_record             
; 2008-09-12T17:39 Initial CIF as created by GSAS2CIF
;

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
;
Common isotropic displacement parameters were used for all heavy atoms
of the fumarate ion. The Uiso values of H atoms were constrained to be
twice the Uiso values of the heavy atoms they are bound to.
Water H atoms were placed in calculated positions and refined in riding
mode. Bond length and bond angle restraints were based on average values
taken from similar structures in the CSD. Planar group restraints were
applied for the ehtenylene and the carboxylate groups.
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/\s(Y~obs~)^2^
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    5

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
# Rietveld study, this information should be moved into the phase
# blocks)

# The following three fields describe the preparation of the material.
# 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               0
_pd_prep_pressure                100
_pd_prep_temperature             298

_pd_char_colour                  white # use ICDD colour descriptions
_refine_ls_shift/su_max          0.03
_refine_ls_shift/su_mean         0.00
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     37
_refine_ls_goodness_of_fit_all   1.36
_refine_ls_number_restraints     16
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
;
zinc fumarate dihydrate
;
_chemical_name_common            'zinc fumarate dihydrate'
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  '-P 2ybc'

_exptl_crystal_F_000             216
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    DASH

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

# 8. Phase information from GSAS

_pd_phase_name                   Zn-fumarate-dihydrate
_cell_length_a                   3.39690(6)
_cell_length_b                   10.34413(24)
_cell_length_c                   8.80754(16)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.5452(22)
_cell_angle_gamma                90.0
_cell_volume                     308.031(14)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y+1/2,-z+1/2
-1 -x,-y,-z
-2 +x,-y+1/2,+z+1/2

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Zn Zn1 0.0 0.5 0.0 1.0 Uiso 0.04216 2
O O2 0.3185(7) 0.68206(25) 0.28661(29) 1.0 Uiso 0.0398 4
O O3 0.0429(7) 0.49427(29) 0.21892(19) 1.0 Uiso 0.0398 4
O O4 0.4934(12) 0.63675(30) 0.0046(4) 1.0 Uiso 0.04831 4
C C5 0.1513(4) 0.57952(18) 0.31528(15) 1.0 Uiso 0.0398 4
C C6 0.0740(4) 0.55275(7) 0.47574(10) 1.0 Uiso 0.0398 4
H H7 0.1413(11) 0.62057(22) 0.54624(23) 1.0 Uiso 0.07959 4
H H9 0.5162(12) 0.68922(30) 0.0981(4) 1.0 Uiso 0.09663 4
H H10 0.4703(12) 0.69392(30) -0.0849(4) 1.0 Uiso 0.09663 4

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C4 H6 O6 Zn'
_chemical_formula_weight         215.47
_cell_formula_units_Z            2

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O3 1.9205(17) . 1_555 N
Zn1 O4 2.231(4) . 1_455 N
Zn1 O4 2.191(4) . 1_555 N
O2 C5 1.2407(18) . 1_555 N
O3 C5 1.2542(13) . 1_555 N
O4 H9 0.982850(10) . 1_555 N
O4 H10 0.982680(10) . 1_555 N
C5 C6 1.4882(7) . 1_555 N
C6 C6 1.2913(13) . -1_566 N
C6 H7 0.9500(7) . 1_555 N
H9 O4 0.982850(10) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O3 179.9802 1_555 . -1_565 N
O3 Zn1 O4 89.16(12) 1_555 . 1_455 N
O3 Zn1 O4 91.01(12) 1_555 . 1_555 N
O3 Zn1 O4 88.99(12) 1_555 . -1_565 N
O3 Zn1 O4 90.84(12) 1_555 . -1_665 N
O4 Zn1 O4 100.39(12) 1_455 . 1_555 N
O4 Zn1 O4 79.61(12) 1_455 . -1_565 N
O4 Zn1 O4 179.9515 1_455 . -1_665 N
O4 Zn1 O4 180.0 1_555 . -1_565 N
Zn1 O3 C5 130.28(17) 1_555 . 1_555 N
Zn1 O4 Zn1 100.39(12) 1_555 . 1_655 N
Zn1 O4 H9 111.74(10) 1_555 . 1_555 N
Zn1 O4 H10 111.85(9) 1_555 . 1_555 N
Zn1 O4 H9 111.52(9) 1_655 . 1_555 N
Zn1 O4 H10 111.65(9) 1_655 . 1_555 N
H9 O4 H10 109.4837(16) 1_555 . 1_555 N
O2 C5 O3 125.00(8) 1_555 . 1_555 N
O2 C5 C6 118.60(8) 1_555 . 1_555 N
O3 C5 C6 116.40(7) 1_555 . 1_555 N
C5 C6 C6 125.556(30) 1_555 . -1_566 N
C5 C6 H7 115.45(5) 1_555 . 1_555 N
C6 C6 H7 118.99(6) -1_566 . 1_555 N

# Powder diffraction data for histogram 1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
Data below 2theta = 8.0 deg. was excluded because of the strongly curved
background in this region. No peaks were apparent in the excluded region.
;

# 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
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_measurement_device_type  'Philips Xpert Pro'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder'
# 'flat_sheet' or 'irregular'

loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Zn 2.0 0.000 0.000 14.0743 3.26550 7.03180 0.23330 5.16520 10.3163 2.41000
58.7097 1.30410 International_Tables_Vol_C
O 12.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
C 8.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
H 12.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.518
_diffrn_radiation_wavelength     1.5406
_diffrn_radiation_type           'Cu K\a~1~'
_pd_proc_ls_prof_R_factor        0.0532
_pd_proc_ls_prof_wR_factor       0.0743
_pd_proc_ls_prof_wR_expected     0.0562
_refine_ls_R_Fsqd_factor         0.04261

_pd_proc_ls_background_function  
; GSAS Background function number 1 with 8 terms.
Shifted Chebyshev function of 1st kind
1: 234.798 2: -204.380 3: 91.2908 4: -25.3061
5: 7.02810 6: 1.27026 7: -6.14001 8: 8.96791
;

_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 3
Surface roughness abs. correction (Suortti)
Terms = 0.079388 0.16998
Correction is refined.
;
_exptl_absorpt_correction_T_min  0.33857
_exptl_absorpt_correction_T_max  0.86478

_pd_proc_ls_pref_orient_corr     
; March-Dollase
AXIS 1 Ratio= 0.885 Frac 0.611 h= 0.000 k= 1.000 l= 0.000
AXIS 2 Ratio= 0.900 Frac 0.389 h= 0.000 k= 0.000 l= 1.000
Prefered orientation correction range: Min= 0.84210, Max= 1.21331
;

_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 350.320 #2(GV) = 0.000 #3(GW) = 0.886
#4(GP) = 0.000 #5(LX) = 0.000 #6(LY) = 22.761
#7(S/L) = 0.0137 #8(H/L) = 0.0306
#9(trns) = 10.14 #10(shft)= -0.8793
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0030 times the peak
;
_pd_proc_ls_peak_cutoff          0.00300
_pd_proc_info_datetime           2008-09-12T17:39:14
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        4.00419
_pd_meas_2theta_range_max        59.98606
_pd_meas_2theta_range_inc        0.00837
_pd_proc_2theta_range_min        4.00413
_pd_proc_2theta_range_max        59.986
_pd_proc_2theta_range_inc        0.00837

_reflns_number_total             87
_reflns_limit_h_min              0
_reflns_limit_h_max              2
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              -5
_reflns_limit_l_max              5
_reflns_d_resolution_high        1.545
_reflns_d_resolution_low         6.688

_vrf_PLAT731_1.2H2O              
;
PROBLEM: Bond Calc 0.983(5), Rep 0.98285(1) ...... 9.90 su-Ra
RESPONSE: The checkcif routine neglects the co-variance matrix and the
restraints employed. These have been accounted for in our calculations.
;

_vrf_PLAT732_1.2H2O              
;
PROBLEM: Angle Calc 109.6(4), Rep 109.48 ...... 9.90 su-Ra
RESPONSE: The checkcif routine neglects the co-variance matrix and the
restraints employed. These have been accounted for in our calculations.
;

data_3
_database_code_depnum_ccdc_archive 'CCDC 707190'

_pd_block_id                     
2008-10-02T14:55|RIET2|L_Fabian|Philips_Xpert_Pro

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2008-10-02T14:55
_audit_author_name               'L Fabian'
_audit_update_record             
; 2008-10-02T14:55 Initial CIF as created by GSAS2CIF
;

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
;
Common isotropic displacement parameters were used for all heavy atoms
within both the fumarate and bipyridylethene fragments.
The Uiso values of H atoms were constrained to be 2 times the Uiso values
of the heavy atoms they are bound to.
Bond length and bond angle restraints were based on average values taken
from similar structures in the CSD. Planar group restraints were applied
for the pyridine rings, the ehtenylene and the carboxylate groups.
;

_pd_proc_ls_special_details      
;
Empirical anisotropic broadening was included in the profile function.
The need for this was indicated by the width of the 020 peak, which is
approx. twice as wide as neighbouring peaks.
The Le Bail fit gave chi^2^ = 7.
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/\s(Y~obs~)^2^
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    2

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
# Rietveld study, this information should be moved into the phase
# blocks)

# The following three fields describe the preparation of the material.
# 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               0
_pd_prep_pressure                100
_pd_prep_temperature             298

_pd_char_colour                  white # use ICDD colour descriptions
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     81
_refine_ls_goodness_of_fit_all   4.14
_refine_ls_number_restraints     71
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
;
zinc(trans-1,2-bis(4-pyridyl)ethylene) fumarate
;
_chemical_name_common            
'zinc(trans-1,2-bis(4-pyridyl)ethylene) fumarate'
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  '-C 2yc'

_exptl_crystal_F_000             1088
_exptl_crystal_density_diffrn    1.5244(2)
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    'coordinates from isostructural Cu-framework'

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

# 8. Phase information from GSAS

_pd_phase_name                   Zn-fumarate-bpe
_cell_length_a                   16.4332(9)
_cell_length_b                   10.7749(9)
_cell_length_c                   13.7840(12)
_cell_angle_alpha                90.0
_cell_angle_beta                 104.979(7)
_cell_angle_gamma                90.0
_cell_volume                     2357.7(4)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y,-z+1/2
-1 -x,-y,-z
-2 +x,-y,+z+1/2
101 +x+1/2,+y+1/2,+z
102 -x+1/2,+y+1/2,-z+1/2
-101 -x+1/2,-y+1/2,-z
-102 +x+1/2,-y+1/2,+z+1/2

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Zn Zn1 0.34426(16) 0.7547(6) 0.51487(28) 1.0 Uiso 0.10123 8
O O2 0.3154(7) 0.5966(10) 0.4207(7) 1.0 Uiso 0.08443 8
O O3 0.1778(7) 0.5882(12) 0.4126(8) 1.0 Uiso 0.08443 8
C C4 0.2396(7) 0.5676(7) 0.3790(5) 1.0 Uiso 0.08443 8
C C5 0.2236(6) 0.4950(6) 0.2841(5) 1.0 Uiso 0.08443 8
H H6 0.1673(6) 0.4749(13) 0.2495(8) 1.0 Uiso 0.16886 8
C C7 0.2861(6) 0.4534(7) 0.2493(5) 1.0 Uiso 0.08443 8
H H8 0.3423(6) 0.4722(13) 0.2853(9) 1.0 Uiso 0.16886 8
C C9 0.2722(6) 0.3747(6) 0.1577(5) 1.0 Uiso 0.08443 8
O O10 0.3344(6) 0.3573(10) 0.1238(7) 1.0 Uiso 0.08443 8
O O11 0.1979(6) 0.3397(10) 0.1179(7) 1.0 Uiso 0.08443 8
N N12 0.46687(26) 0.7641(12) 0.5179(7) 1.0 Uiso 0.08832 8
C C13 0.50269(27) 0.6760(11) 0.4757(6) 1.0 Uiso 0.08832 8
H H14 0.4677(4) 0.6122(12) 0.4396(10) 1.0 Uiso 0.17663 8
C C15 0.58754(27) 0.6735(7) 0.4784(5) 1.0 Uiso 0.08832 8
H H16 0.6091(4) 0.6104(8) 0.4439(7) 1.0 Uiso 0.17663 8
C C17 0.63927(23) 0.7675(6) 0.5263(5) 1.0 Uiso 0.08832 8
C C18 0.6035(4) 0.8553(7) 0.5755(5) 1.0 Uiso 0.08832 8
H H19 0.6370(5) 0.9205(7) 0.6115(8) 1.0 Uiso 0.17663 8
C C20 0.5174(4) 0.8532(10) 0.5663(8) 1.0 Uiso 0.08832 8
H H21 0.4940(6) 0.9149(13) 0.6004(10) 1.0 Uiso 0.17663 8
C C22 0.73036(15) 0.7751(6) 0.53251(28) 1.0 Uiso 0.08832 8
H H23 0.76401(30) 0.8225(18) 0.5862(11) 1.0 Uiso 0.17663 8

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C10 H7 N O4 Zn'
_chemical_formula_weight         270.55
_cell_formula_units_Z            8

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 Zn1 3.020(5) . -101_456 N
Zn1 O2 2.120(10) . 1_555 N
Zn1 O3 2.046(9) . -101_456 N
Zn1 O10 1.965(7) . -2_565 N
Zn1 O11 2.003(8) . 102_555 N
Zn1 N12 2.007(4) . 1_555 N
O2 C4 1.268(4) . 1_555 N
O3 C4 1.240(4) . 1_555 N
C4 C5 1.4885(20) . 1_555 N
C5 H6 0.9499(21) . 1_555 N
C5 C7 1.3201(20) . 1_555 N
C7 H8 0.9499(21) . 1_555 N
C7 C9 1.4884(20) . 1_555 N
C9 O10 1.243(4) . 1_555 N
C9 O11 1.261(4) . 1_555 N
N12 C13 1.3275(19) . 1_555 N
N12 C20 1.3303(19) . 1_555 N
C13 H14 0.9503(21) . 1_555 N
C13 C15 1.3856(18) . 1_555 N
C15 H16 0.9497(21) . 1_555 N
C15 C17 1.3758(19) . 1_555 N
C17 C18 1.3810(19) . 1_555 N
C17 C22 1.4792(20) . 1_555 N
C18 H19 0.9503(21) . 1_555 N
C18 C20 1.3880(18) . 1_555 N
C20 H21 0.9505(21) . 1_555 N
C22 C22 1.346(4) . -101_556 N
C22 H23 0.9505(21) . 1_555 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O3 157.59(25) 1_555 . -101_455 N
O2 Zn1 O10 85.7(6) 1_555 . -2_566 N
O2 Zn1 O11 80.7(4) 1_555 . 102_555 N
O2 Zn1 N12 96.8(6) 1_555 . 1_555 N
O3 Zn1 O10 94.3(5) -101_566 . -2_566 N
O3 Zn1 O11 90.3(6) -101_566 . 102_555 N
O3 Zn1 N12 104.6(6) -101_566 . 1_555 N
O10 Zn1 O11 154.4(4) -2_566 . 102_555 N
O10 Zn1 N12 107.2(4) -2_566 . 1_555 N
O11 Zn1 N12 96.0(4) 102_555 . 1_555 N
Zn1 O2 C4 120.9(6) 1_555 . 1_555 N
Zn1 O3 C4 126.6(7) -101_566 . 1_555 N
O2 C4 O3 126.17(14) 1_555 . 1_555 N
O2 C4 C5 117.23(23) 1_555 . 1_555 N
O3 C4 C5 116.48(24) 1_555 . 1_555 N
C4 C5 H6 119.28(14) 1_555 . 1_555 N
C4 C5 C7 121.36(8) 1_555 . 1_555 N
H6 C5 C7 119.29(10) 1_555 . 1_555 N
C5 C7 H8 118.69(12) 1_555 . 1_555 N
C5 C7 C9 122.59(10) 1_555 . 1_555 N
H8 C7 C9 118.69(12) 1_555 . 1_555 N
C7 C9 O10 116.37(24) 1_555 . 1_555 N
C7 C9 O11 117.29(23) 1_555 . 1_555 N
O10 C9 O11 126.13(15) 1_555 . 1_555 N
Zn1 O10 C9 128.2(4) -2_565 . 1_555 N
Zn1 O11 C9 127.0(4) 102_545 . 1_555 N
Zn1 N12 C13 120.7(6) 1_555 . 1_555 N
Zn1 N12 C20 122.7(6) 1_555 . 1_555 N
C13 N12 C20 116.49(16) 1_555 . 1_555 N
N12 C13 H14 118.00(20) 1_555 . 1_555 N
N12 C13 C15 123.99(10) 1_555 . 1_555 N
H14 C13 C15 117.98(20) 1_555 . 1_555 N
C13 C15 H16 120.26(11) 1_555 . 1_555 N
C13 C15 C17 119.44(8) 1_555 . 1_555 N
H16 C15 C17 120.18(19) 1_555 . 1_555 N
C15 C17 C18 116.80(14) 1_555 . 1_555 N
C15 C17 C22 123.99(8) 1_555 . 1_555 N
C18 C17 C22 119.11(7) 1_555 . 1_555 N
C17 C18 H19 120.02(19) 1_555 . 1_555 N
C17 C18 C20 119.84(7) 1_555 . 1_555 N
H19 C18 C20 119.98(14) 1_555 . 1_555 N
N12 C20 C18 123.13(10) 1_555 . 1_555 N
N12 C20 H21 118.29(20) 1_555 . 1_555 N
C18 C20 H21 118.40(12) 1_555 . 1_555 N
C17 C22 C22 126.27(7) 1_555 . -101_666 N
C17 C22 H23 116.82(22) 1_555 . 1_555 N
C22 C22 H23 116.86(27) -101_666 . 1_555 N

# Powder diffraction data for histogram 1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
Data below 2theta = 8.0 deg. was excluded because of the strongly curved
background in this region. No peaks were apparent in the excluded region.
;

# 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
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              ?
_diffrn_measurement_device_type  'Philips Xpert Pro'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder'
# 'flat_sheet' or 'irregular'

loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Zn 8.0 0.000 0.000 14.0743 3.26550 7.03180 0.23330 5.16520 10.3163 2.41000
58.7097 1.30410 International_Tables_Vol_C
O 32.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
C 80.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
H 56.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
N 8.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.48
_diffrn_radiation_wavelength     1.5406
_diffrn_radiation_type           'Cu K\a~1~'
_pd_proc_ls_prof_R_factor        0.0539
_pd_proc_ls_prof_wR_factor       0.0676
_pd_proc_ls_prof_wR_expected     0.0166
_refine_ls_R_Fsqd_factor         0.05911

_pd_proc_ls_background_function  
; GSAS Background function number 1 with 4 terms.
Shifted Chebyshev function of 1st kind
1: 2513.28 2: -2015.62 3: 852.121 4: -199.417
;

_exptl_absorpt_process_details   
; GSAS Absorption/surface roughness correction: function number 3
Surface roughness abs. correction (Suortti)
Terms = 0.090671 0.34147
Correction is refined.
;
_exptl_absorpt_correction_T_min  0.14674
_exptl_absorpt_correction_T_max  0.80314

_pd_proc_ls_profile_function     
;
CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 1130.890 #2(GV) = 0.000 #3(GW) = 19.132
#4(GP) = 0.000 #5(LX) = 0.000 #6(LY) = 96.498
#7(S/L) = 0.0112 #8(H/L) = 0.0307
#9(trns) = -13.48 #10(shft)= -1.8642
#11(stec)= 0.00 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = -0.146 #15(L22) = 1.002 #16(L33) = 0.330
#17(L12) = -0.238 #18(L13) = 0.388 #19(L23) = -0.708
Peak tails are ignored where the intensity is below 0.0010 times the peak
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_info_datetime           2008-10-02T14:55:06
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        4.00419
_pd_meas_2theta_range_max        59.98607
_pd_meas_2theta_range_inc        0.00837
_pd_proc_2theta_range_min        4.00419
_pd_proc_2theta_range_max        59.98607
_pd_proc_2theta_range_inc        0.00837

_pd_meas_number_of_points        6687
_pd_proc_number_of_points        6687

_reflns_number_total             335
_reflns_limit_h_min              0
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              8
_reflns_limit_l_min              -10
_reflns_limit_l_max              9
_reflns_d_resolution_high        1.549
_reflns_d_resolution_low         8.915

_vrf_PLAT731_3                   
;
PROBLEM: Bond Calc 1.488(10), Rep 1.489(2) ...... 5.00 su-Ra
RESPONSE: The checkcif routine neglects the co-variance matrix and the
restraints employed. These have been accounted for in our calculations.
;

_vrf_PLAT732_3                   
;
PROBLEM: Angle Calc 121.4(9), Rep 121.36(8) ...... 9.90 su-Ra
RESPONSE: The checkcif routine neglects the co-variance matrix and the
restraints employed. These have been accounted for in our calculations.
;