#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:20:47 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185219 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/51/7225148.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7225148
loop_
_publ_author_name
'Xie, Kai-Ping'
'Xu, Wei-Jian'
'He, Chun-Ting'
'Huang, Bo'
'Du, Zi-Yi'
'Su, Yu-Jun'
'Zhang, Wei-Xiong'
'Chen, Xiao-Ming'
_publ_section_title
;
 Order--disorder phase transition in the first thiocyanate-bridged double
 perovskite-type coordination polymer: [NH4]2[NiCd(SCN)6]
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4495
_journal_paper_doi               10.1039/C6CE00898D
_journal_volume                  18
_journal_year                    2016
_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
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-14 deposited with the CCDC.
2016-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.283(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7174(19)
_cell_length_b                   8.617(2)
_cell_length_c                   12.019(3)
_cell_measurement_reflns_used    2275
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     901.4(4)
_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)'
_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_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_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.047
_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
_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_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0457
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1644
_reflns_number_total             2042
_reflns_threshold_expression     'I > 2σ(I)'
_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
  
  
;
_cod_data_source_file            c6ce00898d4.cif
_cod_data_source_block           90k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7225148--7225149.cif.
;
_cod_original_cell_volume        901.4(3)
_cod_database_code               7225148
_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.
;
_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)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
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'
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
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)
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'
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
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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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
