# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_90k
_database_code_depnum_ccdc_archive 'CCDC 1473989'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_audit_creation_date             2016-03-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C12 Cd2 N12 Ni2 S12), 2(H4 N)'
_chemical_formula_sum            'C6 H8 Cd N8 Ni S6'
_chemical_formula_weight         555.67
_chemical_melting_point          ?
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'
Ni Ni 0.3393 1.1124 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7174(19)
_cell_length_b                   8.617(2)
_cell_length_c                   12.019(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.283(6)
_cell_angle_gamma                90
_cell_volume                     901.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   None
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6651
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         3.327
_diffrn_ambient_temperature      90
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
scan:
	Number of images: 282
	           Slice: -63.0000 - 78.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 108.0000
	             XTD: 45.2202
	          2theta: 13.2015
scan:
	Number of images: 122
	           Slice: -12.0000 - 49.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: -36.0000
	             XTD: 45.2202
	          2theta: 13.2015
scan:
	Number of images: 142
	           Slice: -11.0000 - 60.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: 108.0000
	             XTD: 45.2202
	          2theta: 13.2015
scan:
	Number of images: 122
	           Slice: -25.0000 - 36.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -108.0000
	             XTD: 45.2202
	          2theta: 13.2015
scan:
	Number of images: 29
	           Slice: -51.0000 - -36.5000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 36.0000
	             XTD: 45.2202
	          2theta: 13.2015
;
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Pilatus 300K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.055666
_diffrn_orient_matrix_UB_12      -0.090752
_diffrn_orient_matrix_UB_13      -0.043536
_diffrn_orient_matrix_UB_21      -0.086749
_diffrn_orient_matrix_UB_22      -0.017178
_diffrn_orient_matrix_UB_23      -0.075110
_diffrn_orient_matrix_UB_31      0.040126
_diffrn_orient_matrix_UB_32      0.045697
_diffrn_orient_matrix_UB_33      -0.056795
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1644
_reflns_number_total             2042
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.312
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       0.0142(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2042
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1037
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
2.a Riding coordinates:
 N4(H4A,H4B,H4C,H4D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cd1 Cd 0.5000 0.5000 0.5000 0.01006(16) Uani 1 2 d S T P . .
Ni1 Ni 0.0000 1.0000 0.5000 0.0090(2) Uani 1 2 d S T P . .
S1 S 0.28203(12) 0.55036(13) 0.64731(9) 0.0135(3) Uani 1 1 d . . . . .
S2 S 0.73777(12) 0.56752(13) 0.64749(9) 0.0150(3) Uani 1 1 d . . . . .
S3 S 0.51241(12) 0.20249(12) 0.56717(10) 0.0160(3) Uani 1 1 d . . . . .
N1 N 0.1065(4) 0.7941(4) 0.5489(3) 0.0151(8) Uani 1 1 d . . . . .
N2 N 0.5892(4) 0.5222(4) 0.8460(3) 0.0155(8) Uani 1 1 d . . . . .
N3 N 0.1999(4) 0.1183(4) 0.5523(3) 0.0141(8) Uani 1 1 d . . . . .
C1 C 0.1769(5) 0.6927(5) 0.5874(3) 0.0123(9) Uani 1 1 d . . . . .
C2 C 0.6513(5) 0.5370(5) 0.7655(4) 0.0120(9) Uani 1 1 d . . . . .
C3 C 0.3269(5) 0.1557(5) 0.5579(3) 0.0122(9) Uani 1 1 d . . . . .
N4 N 0.0192(4) 0.3626(5) 0.7730(3) 0.0239(9) Uani 1 1 d . . . . .
H4A H 0.0969 0.4082 0.7427 0.029 Uiso 1 1 d R . . . .
H4B H 0.0396 0.2629 0.7790 0.029 Uiso 1 1 d R . . . .
H4C H 0.0103 0.4027 0.8397 0.029 Uiso 1 1 d R . . . .
H4D H -0.0693 0.3735 0.7347 0.029 Uiso 1 1 d R . . . .

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
Cd1 0.0109(2) 0.0105(3) 0.0086(3) -0.00058(15) -0.00077(18) 0.00006(15)
Ni1 0.0086(4) 0.0106(4) 0.0079(4) 0.0008(3) 0.0002(3) -0.0001(3)
S1 0.0138(5) 0.0156(6) 0.0113(6) 0.0031(4) 0.0014(4) 0.0032(4)
S2 0.0122(5) 0.0237(6) 0.0091(6) 0.0015(4) -0.0004(4) -0.0023(4)
S3 0.0102(5) 0.0123(5) 0.0249(7) 0.0035(5) -0.0032(4) -0.0010(4)
N1 0.0135(18) 0.0142(19) 0.018(2) 0.0039(15) 0.0023(15) 0.0009(14)
N2 0.0115(18) 0.0205(19) 0.014(2) -0.0036(15) -0.0026(16) -0.0014(14)
N3 0.0136(18) 0.018(2) 0.0108(19) 0.0010(15) -0.0012(15) -0.0019(14)
C1 0.013(2) 0.015(2) 0.009(2) -0.0021(17) 0.0034(17) -0.0019(16)
C2 0.0085(19) 0.0124(19) 0.015(2) -0.0011(17) -0.0019(17) 0.0003(16)
C3 0.017(2) 0.011(2) 0.008(2) -0.0009(16) -0.0007(17) 0.0003(16)
N4 0.018(2) 0.018(2) 0.036(3) 0.0067(19) 0.0023(18) -0.0039(15)

_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
Cd1 S1 2.7054(11) 3_666 ?
Cd1 S1 2.7054(11) . ?
Cd1 S2 2.7122(12) . ?
Cd1 S2 2.7122(12) 3_666 ?
Cd1 S3 2.6881(12) 3_666 ?
Cd1 S3 2.6881(12) . ?
Ni1 N1 2.072(4) . ?
Ni1 N1 2.072(4) 3_576 ?
Ni1 N2 2.058(4) 4_575 ?
Ni1 N2 2.058(4) 2_556 ?
Ni1 N3 2.084(4) 3_566 ?
Ni1 N3 2.084(4) 1_565 ?
S1 C1 1.669(4) . ?
S2 C2 1.665(5) . ?
S3 C3 1.664(4) . ?
N1 C1 1.150(5) . ?
N2 Ni1 2.058(4) 2_546 ?
N2 C2 1.142(6) . ?
N3 Ni1 2.084(4) 1_545 ?
N3 C3 1.152(5) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8802 . ?
N4 H4C 0.8800 . ?
N4 H4D 0.8800 . ?

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
S1 Cd1 S1 180.0 3_666 . ?
S1 Cd1 S2 85.59(4) 3_666 . ?
S1 Cd1 S2 94.41(4) . . ?
S1 Cd1 S2 94.41(4) 3_666 3_666 ?
S1 Cd1 S2 85.59(4) . 3_666 ?
S2 Cd1 S2 180.0 . 3_666 ?
S3 Cd1 S1 88.52(3) 3_666 3_666 ?
S3 Cd1 S1 91.48(3) 3_666 . ?
S3 Cd1 S1 91.48(3) . 3_666 ?
S3 Cd1 S1 88.52(3) . . ?
S3 Cd1 S2 90.45(3) 3_666 . ?
S3 Cd1 S2 89.55(3) 3_666 3_666 ?
S3 Cd1 S2 89.55(3) . . ?
S3 Cd1 S2 90.45(3) . 3_666 ?
S3 Cd1 S3 180.0 3_666 . ?
N1 Ni1 N1 180.00(17) 3_576 . ?
N1 Ni1 N3 88.86(14) 3_576 3_566 ?
N1 Ni1 N3 91.14(14) . 3_566 ?
N1 Ni1 N3 88.86(14) . 1_565 ?
N1 Ni1 N3 91.14(14) 3_576 1_565 ?
N2 Ni1 N1 89.36(14) 4_575 . ?
N2 Ni1 N1 90.64(14) 2_556 . ?
N2 Ni1 N1 90.64(14) 4_575 3_576 ?
N2 Ni1 N1 89.36(14) 2_556 3_576 ?
N2 Ni1 N2 180.0 4_575 2_556 ?
N2 Ni1 N3 92.03(14) 2_556 1_565 ?
N2 Ni1 N3 87.97(15) 4_575 1_565 ?
N2 Ni1 N3 92.03(14) 4_575 3_566 ?
N2 Ni1 N3 87.97(15) 2_556 3_566 ?
N3 Ni1 N3 180.0 3_566 1_565 ?
C1 S1 Cd1 102.97(14) . . ?
C2 S2 Cd1 99.00(16) . . ?
C3 S3 Cd1 100.88(15) . . ?
C1 N1 Ni1 170.1(4) . . ?
C2 N2 Ni1 173.8(4) . 2_546 ?
C3 N3 Ni1 159.8(3) . 1_545 ?
N1 C1 S1 177.7(4) . . ?
N2 C2 S2 177.1(4) . . ?
N3 C3 S3 177.8(4) . . ?
H4A N4 H4B 108.2 . . ?
H4A N4 H4C 108.2 . . ?
H4A N4 H4D 114.1 . . ?
H4B N4 H4C 109.7 . . ?
H4B N4 H4D 108.3 . . ?
H4C N4 H4D 108.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A S1 0.88 2.37 3.248(4) 172.5 .
N4 H4B S1 0.88 2.53 3.312(4) 148.6 2_546
N4 H4D S2 0.88 2.55 3.315(4) 145.2 1_455

_shelx_SHELXL_version_number     2014/7
_iucr_refine_instructions_details 
;

    90k.res created by SHELXL-2014/7

TITL 90K in P21/n #14
CELL 0.71073 8.7174 8.6169 12.0194 90 93.283 90
ZERR 2 0.0019 0.002 0.0026 0 0.006 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cd N Ni S
UNIT 12 16 2 16 2 12
EQIV $1 0.5-X,-0.5+Y,1.5-Z
EQIV $2 -1+X,+Y,+Z
 
L.S. 80
PLAN  2
TEMP -183.15
HTAB N4 S1
HTAB N4 S1_$1
HTAB N4 S2_$2
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\90K.hkl">
REM </olex2.extras>
 
WGHT    0.038000
EXTI    0.014220
FVAR       0.47210
CD1   3    0.500000    0.500000    0.500000    10.50000    0.01090    0.01053 =
         0.00859   -0.00058   -0.00077    0.00006
NI1   5    0.000000    1.000000    0.500000    10.50000    0.00860    0.01055 =
         0.00788    0.00075    0.00016   -0.00013
S1    6    0.282032    0.550363    0.647309    11.00000    0.01380    0.01557 =
         0.01126    0.00315    0.00143    0.00318
S2    6    0.737766    0.567520    0.647486    11.00000    0.01218    0.02367 =
         0.00911    0.00147   -0.00043   -0.00228
S3    6    0.512411    0.202487    0.567170    11.00000    0.01024    0.01227 =
         0.02494    0.00352   -0.00322   -0.00104
N1    4    0.106517    0.794084    0.548852    11.00000    0.01353    0.01418 =
         0.01785    0.00391    0.00231    0.00094
N2    4    0.589207    0.522244    0.845964    11.00000    0.01151    0.02045 =
         0.01406   -0.00362   -0.00258   -0.00142
N3    4    0.199852    0.118342    0.552316    11.00000    0.01360    0.01762 =
         0.01081    0.00101   -0.00120   -0.00193
C1    1    0.176854    0.692655    0.587389    11.00000    0.01278    0.01549 =
         0.00905   -0.00212    0.00338   -0.00186
C2    1    0.651279    0.536982    0.765496    11.00000    0.00852    0.01237 =
         0.01482   -0.00108   -0.00191    0.00034
C3    1    0.326935    0.155698    0.557929    11.00000    0.01728    0.01102 =
         0.00812   -0.00094   -0.00066    0.00034
N4    4    0.019167    0.362645    0.773011    11.00000    0.01772    0.01798 =
         0.03597    0.00673    0.00230   -0.00387
AFIX   3  0.8800
H4A   2    0.096907    0.408185    0.742691    11.00000   -1.20000
H4B   2    0.039597    0.262865    0.779011    11.00000   -1.20000
H4C   2    0.010327    0.402725    0.839681    11.00000   -1.20000
H4D   2   -0.069263    0.373495    0.734701    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  90K in P21/n #14
REM R1 =  0.0457 for    1644 Fo > 4sig(Fo)  and  0.0520 for all    2042 data
REM    104 parameters refined using      0 restraints
 
END  
     
WGHT      0.0380      0.0000 

REM Highest difference peak  2.312,  deepest hole -1.551,  1-sigma level  0.246
Q1    1   0.4994  0.6033  0.4980  11.00000  0.05    2.31
Q2    1   0.5819  0.4955  0.4594  11.00000  0.05    1.40

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0457 for 1644 Fo > 4sig(Fo) and 0.0520 for all 6935 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.31, deepest hole -1.55
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0520
  REM R1_gt = 0.0457
  REM wR_ref = 0.1037
  REM GOOF = 0.965
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 6935
  REM Reflections_gt = 1644
  REM Parameters = n/a
  REM Hole = -1.55
  REM Peak = 2.31
  REM Flack = n/a
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_298k
_database_code_depnum_ccdc_archive 'CCDC 1473990'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_audit_creation_date             2016-03-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C12 Cd2 N12 Ni2 S12), 2(H4 N)'
_chemical_formula_sum            'C6 H8 Cd N8 Ni S6'
_chemical_formula_weight         555.67
_chemical_melting_point          ?
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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'
Ni Ni 0.3393 1.1124 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.7522(4)
_cell_length_b                   8.6342(4)
_cell_length_c                   12.1410(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.136(4)
_cell_angle_gamma                90
_cell_volume                     917.47(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2159
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.872
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8682
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         3.713
_diffrn_ambient_temperature      298
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
scan:
	Number of images: 234
	           Slice: -77.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: -108.0000
	             XTD: 45.2613
	          2theta: 13.1969
scan:
	Number of images: 230
	           Slice: -12.0000 - 103.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: 36.0000
	             XTD: 45.2613
	          2theta: 13.1969
scan:
	Number of images: 137
	           Slice: -12.0000 - 56.5000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: -108.0000
	             XTD: 45.2613
	          2theta: 13.1969
scan:
	Number of images: 120
	           Slice: -11.0000 - 49.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: -180.0000
	             XTD: 45.2613
	          2theta: 13.1969
scan:
	Number of images: 112
	           Slice: -77.0000 - -21.0000
	     Image width: 0.5000
	        Exp time: 100.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 108.0000
	             XTD: 45.2613
	          2theta: 13.1969
;
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Pilatus 300K
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.054958
_diffrn_orient_matrix_UB_12      -0.091081
_diffrn_orient_matrix_UB_13      -0.041712
_diffrn_orient_matrix_UB_21      -0.085852
_diffrn_orient_matrix_UB_22      -0.016923
_diffrn_orient_matrix_UB_23      -0.076162
_diffrn_orient_matrix_UB_31      0.038871
_diffrn_orient_matrix_UB_32      0.048185
_diffrn_orient_matrix_UB_33      -0.054524
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1985
_reflns_number_total             2084
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.077(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2084
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+0.4910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0659
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H,H,H) groups
2. Others
 Sof(N4')=Sof(H4'A)=Sof(H4'B)=Sof(H4'C)=Sof(H4'D)=1-FVAR(1)
 Sof(N4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(H4D)=FVAR(1)
3.a Riding coordinates:
 N4(H4A,H4B,H4C,H4D), N4'(H4'A,H4'B,H4'C,H4'D)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Cd1 Cd 0.5000 0.5000 0.5000 0.02770(11) Uani 1 2 d S T P . .
Ni1 Ni 0.0000 1.0000 0.5000 0.02138(12) Uani 1 2 d S T P . .
S1 S 0.28199(6) 0.56841(6) 0.64981(4) 0.03441(15) Uani 1 1 d . . . . .
S2 S 0.73214(6) 0.57016(7) 0.64093(4) 0.03662(16) Uani 1 1 d . . . . .
S3 S 0.50078(6) 0.20606(6) 0.57897(6) 0.04603(18) Uani 1 1 d . . . . .
N1 N 0.1074(2) 0.7929(2) 0.54055(17) 0.0416(4) Uani 1 1 d . . . . .
N2 N 0.5914(2) 0.5118(2) 0.84388(16) 0.0363(4) Uani 1 1 d . . . . .
N3 N 0.1948(2) 0.1190(2) 0.55102(15) 0.0363(4) Uani 1 1 d . . . . .
C1 C 0.1781(2) 0.6993(2) 0.58373(16) 0.0293(4) Uani 1 1 d . . . . .
C2 C 0.6487(2) 0.5314(2) 0.75994(16) 0.0270(4) Uani 1 1 d . . . . .
C3 C 0.3196(2) 0.1576(2) 0.56198(15) 0.0286(4) Uani 1 1 d . . . . .
N4 N -0.007(3) 0.379(2) 0.7826(15) 0.051(4) Uani 0.29(3) 1 d . . . A 1
H4A H -0.0177 0.2794 0.7944 0.077 Uiso 0.29(3) 1 d R . . A 1
H4B H 0.0736 0.3965 0.7416 0.077 Uiso 0.29(3) 1 d R . . A 1
H4C H -0.0131 0.4299 0.8454 0.077 Uiso 0.29(3) 1 d R . . A 1
H4D H -0.0866 0.4166 0.7463 0.077 Uiso 0.29(3) 1 d R . . A 1
N4' N 0.0105(9) 0.3557(12) 0.7469(15) 0.076(3) Uani 0.71(3) 1 d . . . A 2
H4'A H 0.0915 0.4088 0.7266 0.114 Uiso 0.71(3) 1 d R . . A 2
H4'B H 0.0143 0.3390 0.8183 0.114 Uiso 0.71(3) 1 d R . . A 2
H4'C H 0.0132 0.2705 0.7071 0.114 Uiso 0.71(3) 1 d R . . A 2
H4'D H -0.0689 0.4106 0.7254 0.114 Uiso 0.71(3) 1 d R . . A 2

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
Cd1 0.02575(16) 0.03017(16) 0.02719(15) -0.00350(6) -0.00049(10) 0.00095(6)
Ni1 0.0178(2) 0.0252(2) 0.0212(2) 0.00159(10) 0.00105(15) -0.00037(10)
S1 0.0325(3) 0.0415(3) 0.0293(2) 0.00630(19) 0.00453(19) 0.0101(2)
S2 0.0260(3) 0.0595(4) 0.0244(2) 0.0033(2) 0.00045(18) -0.0056(2)
S3 0.0247(3) 0.0329(3) 0.0804(4) 0.0151(3) -0.0113(3) -0.0043(2)
N1 0.0321(10) 0.0381(10) 0.0548(11) 0.0107(8) 0.0059(8) 0.0068(8)
N2 0.0341(10) 0.0490(11) 0.0257(9) 0.0004(7) 0.0041(8) 0.0059(7)
N3 0.0287(9) 0.0431(10) 0.0369(9) 0.0062(7) -0.0032(7) -0.0090(7)
C1 0.0240(9) 0.0306(9) 0.0334(9) -0.0006(7) 0.0047(7) -0.0001(7)
C2 0.0230(9) 0.0315(9) 0.0264(9) -0.0020(7) -0.0025(7) 0.0030(7)
C3 0.0292(10) 0.0271(9) 0.0294(9) 0.0035(7) -0.0009(7) -0.0016(7)
N4 0.067(10) 0.036(6) 0.052(8) 0.014(4) -0.012(6) 0.017(5)
N4' 0.042(2) 0.039(3) 0.146(8) 0.023(4) 0.017(4) -0.004(2)

_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
Cd1 S1 2.7045(5) . ?
Cd1 S1 2.7045(5) 3_666 ?
Cd1 S2 2.7214(5) . ?
Cd1 S2 2.7214(5) 3_666 ?
Cd1 S3 2.7130(5) . ?
Cd1 S3 2.7130(5) 3_666 ?
Ni1 N1 2.0790(18) . ?
Ni1 N1 2.0790(18) 3_576 ?
Ni1 N2 2.0618(19) 2_556 ?
Ni1 N2 2.0618(19) 4_575 ?
Ni1 N3 2.0835(17) 3_566 ?
Ni1 N3 2.0835(17) 1_565 ?
S1 C1 1.657(2) . ?
S2 C2 1.655(2) . ?
S3 C3 1.652(2) . ?
N1 C1 1.144(3) . ?
N2 Ni1 2.0618(19) 2_546 ?
N2 C2 1.149(3) . ?
N3 Ni1 2.0835(17) 1_545 ?
N3 C3 1.150(3) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8801 . ?
N4 H4C 0.8800 . ?
N4 H4D 0.8799 . ?
N4' H4'A 0.8800 . ?
N4' H4'B 0.8799 . ?
N4' H4'C 0.8801 . ?
N4' H4'D 0.8800 . ?

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
S1 Cd1 S1 180.000(16) . 3_666 ?
S1 Cd1 S2 93.177(16) 3_666 3_666 ?
S1 Cd1 S2 86.823(16) . 3_666 ?
S1 Cd1 S2 86.823(16) 3_666 . ?
S1 Cd1 S2 93.177(16) . . ?
S1 Cd1 S3 91.845(18) . 3_666 ?
S1 Cd1 S3 88.156(18) . . ?
S1 Cd1 S3 88.156(19) 3_666 3_666 ?
S1 Cd1 S3 91.844(18) 3_666 . ?
S2 Cd1 S2 180.0 3_666 . ?
S3 Cd1 S2 90.872(18) . 3_666 ?
S3 Cd1 S2 90.872(18) 3_666 . ?
S3 Cd1 S2 89.128(18) 3_666 3_666 ?
S3 Cd1 S2 89.128(18) . . ?
S3 Cd1 S3 180.0 3_666 . ?
N1 Ni1 N1 180.0 3_576 . ?
N1 Ni1 N3 90.88(8) 3_576 1_565 ?
N1 Ni1 N3 90.88(8) . 3_566 ?
N1 Ni1 N3 89.12(8) 3_576 3_566 ?
N1 Ni1 N3 89.12(8) . 1_565 ?
N2 Ni1 N1 89.93(8) 2_556 3_576 ?
N2 Ni1 N1 90.07(8) 4_575 3_576 ?
N2 Ni1 N1 90.07(8) 2_556 . ?
N2 Ni1 N1 89.93(8) 4_575 . ?
N2 Ni1 N2 180.0 4_575 2_556 ?
N2 Ni1 N3 91.23(7) 2_556 1_565 ?
N2 Ni1 N3 88.77(7) 2_556 3_566 ?
N2 Ni1 N3 88.77(7) 4_575 1_565 ?
N2 Ni1 N3 91.23(7) 4_575 3_566 ?
N3 Ni1 N3 180.00(9) 3_566 1_565 ?
C1 S1 Cd1 102.16(7) . . ?
C2 S2 Cd1 100.00(7) . . ?
C3 S3 Cd1 101.01(7) . . ?
C1 N1 Ni1 163.68(19) . . ?
C2 N2 Ni1 173.50(18) . 2_546 ?
C3 N3 Ni1 162.58(18) . 1_545 ?
N1 C1 S1 177.9(2) . . ?
N2 C2 S2 176.73(19) . . ?
N3 C3 S3 177.75(18) . . ?
H4A N4 H4B 109.8 . . ?
H4A N4 H4C 109.8 . . ?
H4A N4 H4D 111.0 . . ?
H4B N4 H4C 117.0 . . ?
H4B N4 H4D 106.9 . . ?
H4C N4 H4D 102.0 . . ?
H4'A N4' H4'B 109.4 . . ?
H4'A N4' H4'C 105.0 . . ?
H4'A N4' H4'D 105.8 . . ?
H4'B N4' H4'C 113.8 . . ?
H4'B N4' H4'D 114.1 . . ?
H4'C N4' H4'D 108.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4A S2 0.88 2.72 3.445(19) 140.3 2_546
N4 H4B S1 0.88 2.60 3.42(2) 154.6 .
N4 H4C S3 0.88 2.56 3.283(19) 140.4 2_556
N4 H4D S2 0.88 2.43 3.293(16) 167.0 1_455
N4' H4'A S1 0.88 2.36 3.228(8) 170.5 .
N4' H4'D S2 0.88 2.44 3.317(8) 171.5 1_455

_shelx_SHELXL_version_number     2014/7
_iucr_refine_instructions_details 
;

    298k.res created by SHELXL-2014/7

TITL 298K in P21/n #14
CELL 0.71073 8.7522 8.6342 12.141 90 90.136 90
ZERR 2 0.0004 0.0004 0.0006 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cd N Ni S
UNIT 12 16 2 16 2 12
EQIV $1 0.5-X,-0.5+Y,1.5-Z
EQIV $2 -1+X,+Y,+Z
EQIV $3 0.5-X,0.5+Y,1.5-Z
 
L.S. 100
PLAN  2
TEMP 24.85
HTAB N4 S1
HTAB N4 S2_$2
HTAB N4 S2_$1
HTAB N4 S3_$3
HTAB N4' S1
HTAB N4' S2_$2
MORE -1
BOND $H
CONF
fmap 2 53
acta 52
OMIT 0 0 2
REM <olex2.extras>
REM <HklSrc "%.\\298K.hkl">
REM </olex2.extras>
 
WGHT    0.036700    0.491000
EXTI    0.076737
FVAR       0.71594   0.28588
CD1   3    0.500000    0.500000    0.500000    10.50000    0.02575    0.03017 =
         0.02719   -0.00350   -0.00049    0.00095
NI1   5    0.000000    1.000000    0.500000    10.50000    0.01779    0.02520 =
         0.02116    0.00159    0.00105   -0.00037
S1    6    0.281989    0.568413    0.649811    11.00000    0.03247    0.04151 =
         0.02929    0.00630    0.00453    0.01014
S2    6    0.732141    0.570157    0.640926    11.00000    0.02596    0.05949 =
         0.02442    0.00329    0.00045   -0.00561
S3    6    0.500777    0.206059    0.578972    11.00000    0.02468    0.03291 =
         0.08044    0.01513   -0.01135   -0.00433
N1    4    0.107402    0.792861    0.540546    11.00000    0.03209    0.03806 =
         0.05475    0.01066    0.00585    0.00679
N2    4    0.591440    0.511830    0.843879    11.00000    0.03409    0.04904 =
         0.02567    0.00042    0.00411    0.00590
N3    4    0.194790    0.119013    0.551018    11.00000    0.02874    0.04309 =
         0.03694    0.00617   -0.00320   -0.00904
C1    1    0.178059    0.699317    0.583726    11.00000    0.02404    0.03060 =
         0.03337   -0.00062    0.00470   -0.00010
C2    1    0.648706    0.531401    0.759935    11.00000    0.02304    0.03150 =
         0.02644   -0.00201   -0.00252    0.00302
C3    1    0.319599    0.157630    0.561982    11.00000    0.02918    0.02712 =
         0.02937    0.00345   -0.00094   -0.00156
PART 1
N4    4   -0.007494    0.379460    0.782606    21.00000    0.06661    0.03568 =
         0.05167    0.01384   -0.01174    0.01699
AFIX   3  0.8800
H4A   2   -0.017714    0.279450    0.794436    21.00000   -1.50000
H4B   2    0.073616    0.396470    0.741646    21.00000   -1.50000
H4C   2   -0.013104    0.429900    0.845446    21.00000   -1.50000
H4D   2   -0.086554    0.416570    0.746306    21.00000   -1.50000
AFIX   0
 
PART 0
PART 2
N4'   4    0.010483    0.355660    0.746861   -21.00000    0.04227    0.03949 =
         0.14560    0.02348    0.01658   -0.00393
AFIX   3  0.8800
H4'A  2    0.091513    0.408780    0.726631   -21.00000   -1.50000
H4'B  2    0.014323    0.338980    0.818311   -21.00000   -1.50000
H4'C  2    0.013193    0.270510    0.707071   -21.00000   -1.50000
H4'D  2   -0.068897    0.410590    0.725441   -21.00000   -1.50000
AFIX   0
HKLF 4
 
REM  298K in P21/n #14
REM R1 =  0.0255 for    1985 Fo > 4sig(Fo)  and  0.0265 for all    2084 data
REM    114 parameters refined using      0 restraints
 
END  
     
WGHT      0.0361      0.3531 

REM Highest difference peak  0.534,  deepest hole -0.697,  1-sigma level  0.125
Q1    1   0.4492  0.2437  0.6244  11.00000  0.05    0.53
Q2    1   0.4759  0.2145  0.5225  11.00000  0.05    0.50

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0255 for 1985 Fo > 4sig(Fo) and 0.0265 for all 8992 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.53, deepest hole -0.70
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0265
  REM R1_gt = 0.0255
  REM wR_ref = 0.0659
  REM GOOF = 1.035
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 8992
  REM Reflections_gt = 1985
  REM Parameters = n/a
  REM Hole = -0.70
  REM Peak = 0.53
  REM Flack = n/a
  
  
;
_olex2_submission_special_instructions 'No special instructions were received'
