# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sb2_p21c
_database_code_depnum_ccdc_archive 'CCDC 1565785'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_date             2017-07-21T11:48:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C10 H18 N4 Na2 O8 S2'
_chemical_formula_moiety         C5H7N2SO3,H2O,Na,C5H7N2SO3,H2O,Na
_chemical_formula_weight         432.38

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.883(7)
_cell_length_b                   5.585(4)
_cell_length_c                   10.779(10)
_cell_angle_alpha                90
_cell_angle_beta                 108.170(10)
_cell_angle_gamma                90
_cell_volume                     908.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2379
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      26

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needles
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             448

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;SADABS
;
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_T_max  0.7462

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       'omega scan acd CCD plate detector'
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_decay_%        none
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_number            7973
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.699
_diffrn_reflns_theta_max         27.054
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_reflns_Friedel_coverage         0
_reflns_number_total             1993
_reflns_number_gt                1445
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²+0.0323P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1993
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.067

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.16768(4) -0.52471(10) 0.41746(6) 0.01959(18) Uani 1 1 d . . . . .
Na2 Na -0.08663(7) -0.04215(18) 0.26763(10) 0.0288(3) Uani 1 1 d . . . . .
O1 O -0.13682(12) -0.2813(3) 0.40606(17) 0.0289(5) Uani 1 1 d . . . . .
O2 O -0.14372(12) -0.6006(3) 0.55297(16) 0.0294(5) Uani 1 1 d . . . . .
O3 O -0.14197(12) -0.6924(3) 0.33357(18) 0.0330(5) Uani 1 1 d . . . . .
O4 O -0.05958(12) -0.4084(3) 0.16293(19) 0.0372(5) Uani 1 1 d . . . . .
H1W H -0.078945 -0.382894 0.088026 0.056 Uiso 1 1 d R U . . .
H2W H -0.086945 -0.509894 0.174026 0.056 Uiso 1 1 d R U . . .
N1 N -0.42236(15) -0.5827(4) 0.2620(2) 0.0303(6) Uani 1 1 d . . . . .
H1N H -0.470969 -0.644092 0.225932 0.036 Uiso 1 1 d R U . . .
N2 N -0.42224(15) -0.3925(4) 0.3420(2) 0.0307(5) Uani 1 1 d . . . . .
C1 C -0.3103(2) -0.1475(5) 0.4983(3) 0.0336(7) Uani 1 1 d . . . . .
H11 H -0.362363 -0.067327 0.504342 0.05 Uiso 1 1 calc R U . . .
H21 H -0.274144 -0.036063 0.469812 0.05 Uiso 1 1 calc R U . . .
H31 H -0.277371 -0.210177 0.582316 0.05 Uiso 1 1 calc R U . . .
C2 C -0.33701(17) -0.3486(4) 0.4021(2) 0.0221(6) Uani 1 1 d . . . . .
C3 C -0.28340(16) -0.5112(4) 0.3604(2) 0.0186(5) Uani 1 1 d . . . . .
C4 C -0.34111(17) -0.6593(4) 0.2704(2) 0.0226(6) Uani 1 1 d . . . . .
C5 C -0.32832(19) -0.8655(5) 0.1903(3) 0.0334(7) Uani 1 1 d . . . . .
H51 H -0.298668 -0.99299 0.246858 0.05 Uiso 1 1 calc R U . . .
H52 H -0.293106 -0.815676 0.136938 0.05 Uiso 1 1 calc R U . . .
H53 H -0.384964 -0.920576 0.135459 0.05 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0201(3) 0.0186(3) 0.0204(3) -0.0018(2) 0.0068(2) -0.0013(3)
Na2 0.0301(6) 0.0285(6) 0.0285(6) 0.0013(4) 0.0102(5) -0.0004(5)
O1 0.0300(11) 0.0247(10) 0.0333(10) -0.0011(8) 0.0119(8) -0.0100(8)
O2 0.0296(11) 0.0315(11) 0.0227(10) 0.0030(8) 0.0017(8) -0.0008(8)
O3 0.0277(11) 0.0342(11) 0.0397(11) -0.0137(9) 0.0140(9) 0.0013(9)
O4 0.0343(12) 0.0317(11) 0.0436(12) 0.0096(9) 0.0093(9) -0.0016(9)
N1 0.0216(13) 0.0309(13) 0.0339(13) -0.0027(10) 0.0021(10) -0.0050(10)
N2 0.0257(13) 0.0312(13) 0.0340(13) 0.0003(10) 0.0076(10) 0.0040(11)
C1 0.0405(18) 0.0265(15) 0.0352(16) -0.0067(12) 0.0140(13) 0.0033(14)
C2 0.0247(15) 0.0202(13) 0.0217(12) 0.0047(10) 0.0075(11) 0.0036(11)
C3 0.0214(13) 0.0157(12) 0.0178(12) 0.0013(10) 0.0049(10) -0.0006(11)
C4 0.0250(15) 0.0216(13) 0.0209(13) 0.0027(10) 0.0068(11) -0.0029(12)
C5 0.0390(18) 0.0299(16) 0.0304(15) -0.0105(12) 0.0092(13) -0.0092(14)


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
S1 O3 1.446(2) . ?
S1 O2 1.453(2) . ?
S1 O1 1.463(2) . ?
S1 C3 1.748(3) . ?
Na2 O1 2.321(2) . ?
Na2 O4 2.330(2) 2 ?
Na2 O3 2.342(2) 1_565 ?
Na2 O2 2.346(3) 4 ?
Na2 O4 2.438(3) . ?
Na2 Na2 4.021(2) 2_545 ?
Na2 Na2 4.021(2) 2 ?
O4 H1W 0.7822 . ?
O4 H2W 0.7463 . ?
N1 C4 1.336(3) . ?
N1 N2 1.367(3) . ?
N1 H1N 0.8232 . ?
N2 C2 1.329(3) . ?
C1 C2 1.497(4) . ?
C1 H11 0.96 . ?
C1 H21 0.96 . ?
C1 H31 0.96 . ?
C2 C3 1.410(3) . ?
C3 C4 1.382(3) . ?
C4 C5 1.491(4) . ?
C5 H51 0.96 . ?
C5 H52 0.96 . ?
C5 H53 0.96 . ?

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
O3 S1 O2 113.77(12) . . ?
O3 S1 O1 112.44(12) . . ?
O2 S1 O1 111.46(11) . . ?
O3 S1 C3 106.20(11) . . ?
O2 S1 C3 106.44(11) . . ?
O1 S1 C3 105.86(11) . . ?
O1 Na2 O4 119.06(8) . 2 ?
O1 Na2 O3 92.76(9) . 1_565 ?
O4 Na2 O3 93.78(8) 2 1_565 ?
O1 Na2 O2 136.47(8) . 4 ?
O4 Na2 O2 104.35(8) 2 4 ?
O3 Na2 O2 87.11(9) 1_565 4 ?
O1 Na2 O4 87.73(9) . . ?
O4 Na2 O4 96.65(6) 2 . ?
O3 Na2 O4 167.78(8) 1_565 . ?
O2 Na2 O4 84.16(9) 4 . ?
O1 Na2 Na2 92.50(6) . 2_545 ?
O4 Na2 Na2 67.05(7) 2 2_545 ?
O3 Na2 Na2 160.18(7) 1_565 2_545 ?
O2 Na2 Na2 102.02(7) 4 2_545 ?
O4 Na2 Na2 31.68(5) . 2_545 ?
O1 Na2 Na2 147.43(7) . 2 ?
O4 Na2 Na2 33.35(6) 2 2 ?
O3 Na2 Na2 77.41(6) 1_565 2 ?
O2 Na2 Na2 74.70(6) 4 2 ?
O4 Na2 Na2 108.32(7) . 2 ?
Na2 Na2 Na2 87.97(6) 2_545 2 ?
S1 O1 Na2 141.23(12) . . ?
S1 O2 Na2 142.35(12) . 4_556 ?
S1 O3 Na2 159.36(13) . 1_545 ?
Na2 O4 Na2 114.97(8) 2_545 . ?
Na2 O4 H1W 114.9 2_545 . ?
Na2 O4 H1W 104.8 . . ?
Na2 O4 H2W 106.1 2_545 . ?
Na2 O4 H2W 111.6 . . ?
H1W O4 H2W 104 . . ?
C4 N1 N2 113.3(2) . . ?
C4 N1 H1N 130 . . ?
N2 N1 H1N 116 . . ?
C2 N2 N1 104.6(2) . . ?
C2 C1 H11 109.5 . . ?
C2 C1 H21 109.5 . . ?
H11 C1 H21 109.5 . . ?
C2 C1 H31 109.5 . . ?
H11 C1 H31 109.5 . . ?
H21 C1 H31 109.5 . . ?
N2 C2 C3 110.5(2) . . ?
N2 C2 C1 120.1(2) . . ?
C3 C2 C1 129.4(2) . . ?
C4 C3 C2 105.9(2) . . ?
C4 C3 S1 127.96(19) . . ?
C2 C3 S1 126.06(18) . . ?
N1 C4 C3 105.7(2) . . ?
N1 C4 C5 120.8(2) . . ?
C3 C4 C5 133.5(2) . . ?
C4 C5 H51 109.5 . . ?
C4 C5 H52 109.5 . . ?
H51 C5 H52 109.5 . . ?
C4 C5 H53 109.5 . . ?
H51 C5 H53 109.5 . . ?
H52 C5 H53 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 O1 Na2 18.8(2) . . . . ?
O2 S1 O1 Na2 147.97(17) . . . . ?
C3 S1 O1 Na2 -96.70(19) . . . . ?
O3 S1 O2 Na2 138.70(18) . . . 4_556 ?
O1 S1 O2 Na2 10.3(2) . . . 4_556 ?
C3 S1 O2 Na2 -104.69(19) . . . 4_556 ?
O2 S1 O3 Na2 5.8(4) . . . 1_545 ?
O1 S1 O3 Na2 133.7(3) . . . 1_545 ?
C3 S1 O3 Na2 -111.0(3) . . . 1_545 ?
C4 N1 N2 C2 0.3(3) . . . . ?
N1 N2 C2 C3 -0.2(3) . . . . ?
N1 N2 C2 C1 179.5(2) . . . . ?
N2 C2 C3 C4 0.0(3) . . . . ?
C1 C2 C3 C4 -179.7(3) . . . . ?
N2 C2 C3 S1 -177.98(18) . . . . ?
C1 C2 C3 S1 2.4(4) . . . . ?
O3 S1 C3 C4 11.0(3) . . . . ?
O2 S1 C3 C4 -110.5(2) . . . . ?
O1 S1 C3 C4 130.8(2) . . . . ?
O3 S1 C3 C2 -171.5(2) . . . . ?
O2 S1 C3 C2 66.9(2) . . . . ?
O1 S1 C3 C2 -51.8(2) . . . . ?
N2 N1 C4 C3 -0.4(3) . . . . ?
N2 N1 C4 C5 180.0(2) . . . . ?
C2 C3 C4 N1 0.2(3) . . . . ?
S1 C3 C4 N1 178.12(18) . . . . ?
C2 C3 C4 C5 179.8(3) . . . . ?
S1 C3 C4 C5 -2.3(4) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1565784'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_iucr_compatibility_tag          ?
#==============================================================================

#data_Compound2

_chemical_name_systematic        
;
?
;
_chemical_name_common            CuLNa*H2O
_chemical_formula_moiety         ?
_chemical_formula_structural     'Cu C5 H8 N2 Na O4 S'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'Cu8 C40 H64 N16 Na8 O32 S8'
_chemical_formula_weight         278.73
_chemical_melting_point          ?
_chemical_compound_source        synthesis

loop_
_atom_type_symbol
_atom_type_description
#   _atom_type_scat_dispersion_real
#   _atom_type_scat_dispersion_imag
_atom_type_scat_source

C C 'International Tables for Crystallography (Vol. IV)'
H H 'International Tables for Crystallography (Vol. IV)'
Cu Cu 'International Tables for Crystallography (Vol. IV)'
N N 'International Tables for Crystallography (Vol. IV)'
O O 'International Tables for Crystallography (Vol. IV)'
S S 'International Tables for Crystallography (Vol. IV)'
Na Na 'International Tables for Crystallography (Vol. IV)'

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

# 1.5. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        C2/c
_space_group_name_Hall           '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'x+1/2, y+1/2, z'

_cell_length_a                   31.61138(54)
_cell_length_b                   5.54791(14)
_cell_length_c                   10.82291(30)
_cell_angle_alpha                90
_cell_angle_beta                 96.9743(20)
_cell_angle_gamma                90
_cell_volume                     1884.046(78)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2016

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              15 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              20 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              1 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
;
packed powder pellet
;
_pd_spec_mount_mode              reflection # options are 'reflection' 
# or 'transmission'

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

_pd_char_particle_morphology     ?
_pd_char_colour                  white # use ICDD colour descriptions



# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    57.8
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

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

# 1.6. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This 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               
; ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_source_target            Cu
_diffrn_source_type              'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Advance'
_diffrn_detector_type            'Bruker Lynxeye position linear PSD'
_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

loop_
_diffrn_radiation_type
'Cu K\a'
_diffrn_radiation_wavelength     CuK\a~1~
_diffrn_radiation_monochromator  'Nickel filter'

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        5001
_pd_meas_2theta_range_min        5
_pd_meas_2theta_range_max        105
_pd_meas_2theta_range_inc        0.02

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?

# The following fields are used to identify the programs used.

_computing_data_collection       'Bruker D8 Command'
_computing_cell_refinement       'Bruker TOPAS-R'
_computing_data_reduction        ?
_computing_structure_solution    'Bruker TOPAS-R'
_computing_structure_refinement  'Bruker TOPAS-R'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

# 1.7. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; 
  
1) The use of a rigid body description for the organic ligand
   does not allow the derivation of statistically meaningful s.u.'s
   for its atoms.
  
   S.u.'s are available only for the center of mass (X, Y, Z), the rotational angles RX, RY, RZ 
   and the rotation about the R(C1, S1)angle:   
  
   X, Y, Z   -0.3851(4), -0.2341(8), 0.9462(4)
   RY, RY, RZ  35.59(34), -303.61(13), 37.32(32)
   R(C1, S1)  -68.77(34)   
  
   for the rigid body described by:
                                                   
rigid                                                                                                                                                                      
S1  ux   0.581772   uy   0.028480   uz   1.660512   
O1  ux  -0.301245   uy  -0.843765   uz   2.410158   
O2  ux   1.933730   uy  -0.491097   uz   1.591590   
O3  ux   0.560679   uy   1.411441   uz   2.095797   
N1  ux  -1.160661   uy  -0.411243   uz  -1.766764   
N2  ux  -0.136816   uy   0.339811   uz  -2.203741   
C1  ux  -0.002099   uy   0.001562   uz   0.017577   
C2  ux  -1.120745   uy  -0.630987   uz  -0.448628   
C3  ux   0.566704   uy   0.591731   uz  -1.113253   
C4  ux   1.859170   uy   1.436177   uz  -1.093772   
C5  ux  -2.137614   uy  -1.441126   uz   0.384192   
H1  ux  -2.575654   uy  -0.803899   uz   1.135490   
H2  ux  -2.912663   uy  -1.818707   uz  -0.263166   
H3  ux  -1.634583   uy  -2.266473   uz   0.861792   
H4  ux   2.675610   uy   0.835208   uz  -0.726828   
H5  ux   2.082564   uy   1.774405   uz  -2.092790   
H6  ux   1.721852   uy   2.288481   uz  -0.448168 

   RY, RY, RZ = rotation angles of the rigid body

;

# The next three items are given as text
_pd_proc_ls_profile_function     'fundamental parameters approach'
_pd_proc_ls_background_function  'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.646
_pd_proc_ls_prof_wR_factor       0.0779
_pd_proc_ls_prof_wR_expected     0.1063

_refine_special_details          
; ?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      1/[Y~i~]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     36
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all   ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          .01
_refine_ls_shift/su_mean         ?


# 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        5
_pd_proc_2theta_range_max        105
_pd_proc_2theta_range_inc        0.02

loop_
_pd_proc_wavelength
1.540562
1.544390

_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     ?

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

# 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Na Na 8 0.71059(15) 0.6897 -0.70853 1 4.676(67)
Ow O 8 -0.78007(22) -0.83565 0.67043 1 4.676(67)
Cu1 Cu 4 0 0 0.5 1 2.676(67)
Cu2 Cu 4 0 -0.65589(72) 0.75 1 2.676(67)
S1 S 8 -0.3293275 -0.2072465 0.9745336 1 4.676(67)
O1 O 8 -0.3197503 -0.1389067 1.104228 1 4.676(67)
O2 O 8 -0.3130743 -0.4447344 0.9501518 1 4.676(67)
O3 O 8 -0.3168972 -0.0295708 0.8875341 1 4.676(67)
N1 N 8 -0.4496931 -0.3552479 0.949728 1 4.676(67)
N2 N 8 -0.4529263 -0.1731103 0.8674025 1 4.676(67)
C1 C 8 -0.3846363 -0.2339918 0.9471581 1 4.676(67)
C2 C 8 -0.4095762 -0.3966353 0.9997582 1 4.676(67)
C3 C 8 -0.4132178 -0.09929019 0.8661792 1 4.676(67)
C4 C 8 -0.400093 0.1103894 0.7850935 1 4.676(67)
C5 C 8 -0.3943701 -0.5902497 1.097662 1 4.676(67)
H1 H 8 -0.3786682 -0.5041856 1.180074 1 4.676(67)
H2 H 8 -0.4214262 -0.6911257 1.121177 1 4.676(67)
H3 H 8 -0.3723978 -0.7106343 1.0601 1 4.676(67)
H4 H 8 -0.3784109 0.04470862 0.723224 1 4.676(67)
H5 H 8 -0.4280504 0.1839556 0.7312318 1 4.676(67)
H6 H 8 -0.3846547 0.2489032 0.8441979 1 4.676(67)
