# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_PBCA
_audit_block_doi                 10.5517/ccdc.csd.cc20y94f
_database_code_depnum_ccdc_archive 'CCDC 1875194'
loop_
_audit_author_name
_audit_author_address
'Dong-Sheng Sun' 'Southeast University'

_audit_update_record             
;
2018-11-22 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd Cl3, C5 H14 N'
_chemical_formula_sum            'C5 H14 Cd Cl3 N'
_chemical_formula_weight         306.93

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

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

_cell_length_a                   16.0893(6)
_cell_length_b                   6.8295(3)
_cell_length_c                   18.8185(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2067.81(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1819
_cell_measurement_theta_min      3.001
_cell_measurement_theta_max      25.020

_exptl_crystal_description       strip
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   0.749
_exptl_transmission_factor_max   0.886
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    2.824
_shelx_estimated_absorpt_T_min   0.330
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_detector                 'CCD plate'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11574
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.508
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1819
_reflns_number_gt                1389
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0775P)²+24.7673P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1818
_refine_ls_number_parameters     95
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0555
_refine_ls_wR_factor_ref         0.1704
_refine_ls_wR_factor_gt          0.1624
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.25037(3) 0.37366(7) 0.37260(3) 0.0291(3) Uani 1 1 d . . . . .
Cl1 Cl 0.12333(12) 0.1245(2) 0.37281(10) 0.0351(5) Uani 1 1 d . . . . .
Cl2 Cl 0.18623(13) 0.6256(2) 0.27837(10) 0.0355(5) Uani 1 1 d . . . . .
Cl3 Cl 0.18793(14) 0.6211(2) 0.46574(10) 0.0387(5) Uani 1 1 d . . . . .
C1 C 0.0340(10) -0.0227(18) 0.1211(7) 0.108(4) Uani 1 1 d D U . . .
H1A H 0.0319 -0.0454 0.0708 0.162 Uiso 1 1 calc R U . . .
H1B H -0.0215 -0.0172 0.1397 0.162 Uiso 1 1 calc R U . . .
H1C H 0.0639 -0.1272 0.1437 0.162 Uiso 1 1 calc R U . . .
C2 C 0.1625(7) 0.119(2) 0.1447(9) 0.117(4) Uani 1 1 d D U . . .
H2A H 0.1679 -0.0046 0.1684 0.175 Uiso 1 1 calc R U . . .
H2B H 0.1879 0.2197 0.1730 0.175 Uiso 1 1 calc R U . . .
H2C H 0.1894 0.1132 0.0993 0.175 Uiso 1 1 calc R U . . .
C3 C 0.0375(6) 0.2612(15) 0.1955(4) 0.059(2) Uani 1 1 d D U . . .
H3A H 0.0469 0.1858 0.2378 0.089 Uiso 1 1 calc R U . . .
H3B H -0.0212 0.2729 0.1873 0.089 Uiso 1 1 calc R U . . .
H3C H 0.0612 0.3892 0.2013 0.089 Uiso 1 1 calc R U . . .
C4 C 0.0585(8) 0.280(2) 0.0714(6) 0.089(3) Uani 1 1 d D U . . .
H4A H -0.0007 0.3060 0.0686 0.107 Uiso 1 1 calc R U . . .
H4B H 0.0745 0.2065 0.0293 0.107 Uiso 1 1 calc R U . . .
C5 C 0.1087(9) 0.4814(17) 0.0742(7) 0.097(5) Uani 1 1 d . . . . .
H5A H 0.0875 0.5609 0.1122 0.145 Uiso 1 1 calc R U . . .
H5B H 0.1022 0.5495 0.0299 0.145 Uiso 1 1 calc R U . . .
H5C H 0.1665 0.4550 0.0823 0.145 Uiso 1 1 calc R U . . .
N1 N 0.0763(4) 0.1635(10) 0.1351(3) 0.0429(15) Uani 1 1 d D 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
Cd1 0.0339(4) 0.0169(4) 0.0365(4) -0.0012(2) 0.0012(2) 0.00034(19)
Cl1 0.0268(10) 0.0258(10) 0.0526(12) -0.0001(8) -0.0023(7) -0.0002(7)
Cl2 0.0437(11) 0.0257(9) 0.0371(10) -0.0013(7) -0.0100(8) -0.0002(8)
Cl3 0.0522(12) 0.0248(9) 0.0390(10) -0.0010(7) 0.0172(9) 0.0005(8)
C1 0.122(7) 0.085(6) 0.117(8) -0.020(5) 0.028(6) -0.020(6)
C2 0.088(6) 0.133(9) 0.129(8) -0.024(6) -0.014(6) 0.035(6)
C3 0.062(6) 0.063(6) 0.053(5) -0.001(4) 0.007(4) -0.003(5)
C4 0.096(5) 0.091(5) 0.081(4) 0.004(4) -0.001(4) 0.007(4)
C5 0.147(13) 0.053(7) 0.091(9) 0.023(6) 0.043(9) -0.013(8)
N1 0.044(4) 0.045(3) 0.040(3) -0.004(3) 0.002(3) -0.001(3)

_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 Cl3 2.6338(18) . ?
Cd1 Cl3 2.6522(18) 8_655 ?
Cd1 Cl2 2.6563(18) 8_655 ?
Cd1 Cl1 2.6579(19) 8_665 ?
Cd1 Cl1 2.6595(19) . ?
Cd1 Cl2 2.6775(18) . ?
Cd1 Cd1 3.41476(15) 8_655 ?
Cd1 Cd1 3.41478(15) 8_665 ?
Cl1 Cd1 2.6579(19) 8_655 ?
Cl2 Cd1 2.6563(18) 8_665 ?
Cl3 Cd1 2.6521(18) 8_665 ?
C1 N1 1.466(9) . ?
C2 N1 1.430(9) . ?
C3 N1 1.459(8) . ?
C4 N1 1.466(8) . ?
C4 C5 1.598(18) . ?

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
Cl3 Cd1 Cl3 96.90(8) . 8_655 ?
Cl3 Cd1 Cl2 179.71(6) . 8_655 ?
Cl3 Cd1 Cl2 83.26(6) 8_655 8_655 ?
Cl3 Cd1 Cl1 82.94(6) . 8_665 ?
Cl3 Cd1 Cl1 97.59(6) 8_655 8_665 ?
Cl2 Cd1 Cl1 96.81(6) 8_655 8_665 ?
Cl3 Cd1 Cl1 96.68(6) . . ?
Cl3 Cd1 Cl1 82.56(6) 8_655 . ?
Cl2 Cd1 Cl1 83.57(6) 8_655 . ?
Cl1 Cd1 Cl1 179.60(7) 8_665 . ?
Cl3 Cd1 Cl2 83.20(6) . . ?
Cl3 Cd1 Cl2 179.22(6) 8_655 . ?
Cl2 Cd1 Cl2 96.65(7) 8_655 . ?
Cl1 Cd1 Cl2 83.20(6) 8_665 . ?
Cl1 Cd1 Cl2 96.66(6) . . ?
Cl3 Cd1 Cd1 129.81(4) . 8_655 ?
Cl3 Cd1 Cd1 49.52(4) 8_655 8_655 ?
Cl2 Cd1 Cd1 50.47(4) 8_655 8_655 ?
Cl1 Cd1 Cd1 130.33(5) 8_665 8_655 ?
Cl1 Cd1 Cd1 50.02(4) . 8_655 ?
Cl2 Cd1 Cd1 129.88(4) . 8_655 ?
Cl3 Cd1 Cd1 49.99(4) . 8_665 ?
Cl3 Cd1 Cd1 130.67(4) 8_655 8_665 ?
Cl2 Cd1 Cd1 129.73(4) 8_655 8_665 ?
Cl1 Cd1 Cd1 50.07(4) 8_665 8_665 ?
Cl1 Cd1 Cd1 129.58(5) . 8_665 ?
Cl2 Cd1 Cd1 49.92(4) . 8_665 ?
Cd1 Cd1 Cd1 179.60(3) 8_655 8_665 ?
Cd1 Cl1 Cd1 79.91(5) 8_655 . ?
Cd1 Cl2 Cd1 79.61(5) 8_665 . ?
Cd1 Cl3 Cd1 80.48(5) . 8_665 ?
N1 C4 C5 109.9(10) . . ?
C2 N1 C3 114.4(9) . . ?
C2 N1 C1 106.9(11) . . ?
C3 N1 C1 109.7(8) . . ?
C2 N1 C4 114.0(10) . . ?
C3 N1 C4 107.9(9) . . ?
C1 N1 C4 103.4(9) . . ?

_refine_diff_density_max         2.041
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.187

_shelx_res_file                  
;

    PBCA.res created by SHELXL-2014/7


TITL PBCA in Pbca
CELL 0.71073  16.0893   6.8295  18.8185  90.000  90.000  90.000
ZERR   8.00   0.0006   0.0003   0.0008   0.000   0.000   0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C  H  N  Cl Cd
UNIT 40 112 8 24 8
OMIT   0.00  50.05
OMIT 3 3 2
L.S. 30
ACTA
BOND
FMAP 2
PLAN 2
DFIX 1.45 0.01 N1 C2 N1 C4 N1 C1 N1 C3
SIMU 0.01 N1 C1 C2 C3 C4
DELU 0.01 N1 C1 C2 C3 C4
ISOR 0.005 C1 C2 C4
TEMP 20
WGHT    0.077500   24.767300
FVAR       0.09326
MOLE 1
CD1   5    0.250366    0.373664    0.372595    11.00000    0.03394    0.01689 =
         0.03653   -0.00122    0.00125    0.00034
CL1   4    0.123329    0.124512    0.372813    11.00000    0.02685    0.02580 =
         0.05256   -0.00008   -0.00234   -0.00020
CL2   4    0.186229    0.625574    0.278368    11.00000    0.04372    0.02566 =
         0.03707   -0.00132   -0.00996   -0.00019
CL3   4    0.187929    0.621082    0.465744    11.00000    0.05220    0.02483 =
         0.03895   -0.00097    0.01721    0.00048
C1    1    0.033996   -0.022660    0.121129    11.00000    0.12183    0.08501 =
         0.11704   -0.01969    0.02789   -0.02034
AFIX 137
H1A   2    0.031914   -0.045404    0.070819    11.00000   -1.50000
H1B   2   -0.021517   -0.017225    0.139727    11.00000   -1.50000
H1C   2    0.063871   -0.127249    0.143696    11.00000   -1.50000
AFIX   0
C2    1    0.162468    0.119318    0.144736    11.00000    0.08808    0.13298 =
         0.12923   -0.02411   -0.01401    0.03544
AFIX 137
H2A   2    0.167921   -0.004583    0.168375    11.00000   -1.50000
H2B   2    0.187930    0.219701    0.173043    11.00000   -1.50000
H2C   2    0.189383    0.113178    0.099262    11.00000   -1.50000
AFIX   0
C3    1    0.037500    0.261208    0.195548    11.00000    0.06234    0.06257 =
         0.05312   -0.00107    0.00723   -0.00256
AFIX 137
H3A   2    0.046902    0.185772    0.237836    11.00000   -1.50000
H3B   2   -0.021177    0.272915    0.187322    11.00000   -1.50000
H3C   2    0.061232    0.389216    0.201252    11.00000   -1.50000
AFIX   0
C4    1    0.058493    0.279556    0.071350    11.00000    0.09584    0.09112 =
         0.08080    0.00407   -0.00060    0.00689
AFIX  23
H4A   2   -0.000652    0.305981    0.068553    11.00000   -1.20000
H4B   2    0.074508    0.206485    0.029324    11.00000   -1.20000
AFIX   0
C5    1    0.108680    0.481394    0.074215    11.00000    0.14710    0.05251 =
         0.09119    0.02349    0.04317   -0.01277
AFIX 137
H5A   2    0.087474    0.560903    0.112176    11.00000   -1.50000
H5B   2    0.102180    0.549470    0.029930    11.00000   -1.50000
H5C   2    0.166528    0.455030    0.082259    11.00000   -1.50000
AFIX   0
N1    3    0.076326    0.163494    0.135096    11.00000    0.04381    0.04511 =
         0.03984   -0.00377    0.00202   -0.00110
HKLF 4

REM  PBCA in Pbca
REM R1 =  0.0555 for    1389 Fo > 4sig(Fo)  and  0.0660 for all    1818 data
REM     95 parameters refined using     56 restraints

END

WGHT      0.0849     18.1779

REM Highest difference peak  2.041,  deepest hole -1.140,  1-sigma level  0.187
Q1    1   0.1491  0.2929  0.1069  11.00000  0.05    2.04
Q2    1   0.0182  0.1239  0.0797  11.00000  0.05    1.93
;
_shelx_res_checksum              83641
####################################################################### 
# 
# 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_p63mmc
_audit_block_doi                 10.5517/ccdc.csd.cc20y95g
_database_code_depnum_ccdc_archive 'CCDC 1875195'
loop_
_audit_author_name
_audit_author_address
'Dong-Sheng Sun'
;Southeast University
China
;
_audit_update_record             
;
2018-12-12 deposited with the CCDC.	2019-03-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(Cd0.33 Cl), C3 N, 2(C H3), 7.92(H)'
_chemical_formula_sum            'C5 H14 Cd Cl3 N'
_chemical_formula_weight         306.85

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           hexagonal
_space_group_IT_number           194
_symmetry_space_group_name_H-M   'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

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

_cell_length_a                   9.5032(3)
_cell_length_b                   9.5032(3)
_cell_length_c                   6.8345(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     534.54(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    363(2)
_cell_measurement_reflns_used    3185
_cell_measurement_theta_min      3.8560
_cell_measurement_theta_max      28.1020

_exptl_crystal_description       strip
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             299.8
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_T_max  0.579
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      363(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6024
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         26.99
_reflns_number_total             253
_reflns_number_gt                216
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0967P)²+0.1085P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         252
_refine_ls_number_parameters     18
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.015

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.59417(2) 0.18834(5) 0.87560(9) 0.206(4) Uani 0.50 2 d SPDU . .
H1A H 0.6458 0.1237 0.8709 0.248 Uiso 0.33 1 d PR . .
H1B H 0.4778 0.1237 0.8709 0.248 Uiso 0.33 1 d PR . .
N1 N 0.6667 0.3333 0.7500 0.155(3) Uani 1 12 d SDU . .
Cd1 Cd 1.0000 0.0000 0.0000 0.07821(16) Uani 1 12 d S . .
Cl1 Cl 0.87623(5) 0.12377(5) 0.2500 0.0989(3) Uani 1 4 d S . .
C2 C 0.6667 0.3333 1.1208(13) 0.50(2) Uani 1 6 d SU . .
H2A H 0.7648 0.3580 1.1887 0.599 Uiso 0.25 1 d PR . .
H2B H 0.5932 0.3580 1.1887 0.599 Uiso 0.25 1 d PR . .

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
C1 0.165(6) 0.159(6) 0.293(8) 0.031(7) 0.015(3) 0.080(3)
N1 0.109(3) 0.109(3) 0.245(8) 0.000 0.000 0.0546(13)
Cd1 0.0782(2) 0.0782(2) 0.0783(3) 0.000 0.000 0.03908(10)
Cl1 0.1150(2) 0.1150(2) 0.0967(6) 0.000 0.000 0.0801(3)
C2 0.64(4) 0.64(4) 0.227(14) 0.000 0.000 0.318(18)

_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
C1 N1 1.4699(4) . ?
C1 C1 1.7169(13) 16_557 ?
C1 H1A 0.9595 . ?
C1 H1B 0.9599 . ?
N1 C1 1.4700(4) 18_667 ?
N1 C1 1.4700(4) 3_665 ?
N1 C1 1.4700(4) 16_557 ?
N1 C1 1.4700(4) 2_655 ?
N1 C1 1.4700(4) 17_657 ?
Cd1 Cl1 2.6590(7) 15_545 ?
Cd1 Cl1 2.6590(7) . ?
Cd1 Cl1 2.6590(7) 14_665 ?
Cd1 Cl1 2.6590(7) 2_645 ?
Cd1 Cl1 2.6590(7) 3_765 ?
Cd1 Cl1 2.6590(7) 13_755 ?
Cd1 Cd1 3.4173(2) 4_754 ?
Cd1 Cd1 3.4173(2) 4_755 ?
Cl1 Cd1 2.6590(7) 4_755 ?
C2 C2 1.766(18) 16_558 ?
C2 H2A 0.9600 . ?
C2 H2B 0.9601 . ?

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
N1 C1 C1 54.27(3) . 16_557 ?
N1 C1 H1A 115.5 . . ?
C1 C1 H1A 88.1 16_557 . ?
N1 C1 H1B 115.5 . . ?
C1 C1 H1B 88.1 16_557 . ?
H1A C1 H1B 112.6 . . ?
C1 N1 C1 132.108(17) . 18_667 ?
C1 N1 C1 89.34(4) . 3_665 ?
C1 N1 C1 71.46(5) 18_667 3_665 ?
C1 N1 C1 71.46(5) . 16_557 ?
C1 N1 C1 89.34(4) 18_667 16_557 ?
C1 N1 C1 132.108(17) 3_665 16_557 ?
C1 N1 C1 89.34(4) . 2_655 ?
C1 N1 C1 132.107(16) 18_667 2_655 ?
C1 N1 C1 89.34(4) 3_665 2_655 ?
C1 N1 C1 132.106(16) 16_557 2_655 ?
C1 N1 C1 132.107(16) . 17_657 ?
C1 N1 C1 89.34(4) 18_667 17_657 ?
C1 N1 C1 132.107(16) 3_665 17_657 ?
C1 N1 C1 89.34(4) 16_557 17_657 ?
C1 N1 C1 71.46(5) 2_655 17_657 ?
Cl1 Cd1 Cl1 96.857(18) 15_545 . ?
Cl1 Cd1 Cl1 83.144(18) 15_545 14_665 ?
Cl1 Cd1 Cl1 96.856(18) . 14_665 ?
Cl1 Cd1 Cl1 96.856(18) 15_545 2_645 ?
Cl1 Cd1 Cl1 83.144(18) . 2_645 ?
Cl1 Cd1 Cl1 180.0 14_665 2_645 ?
Cl1 Cd1 Cl1 180.0 15_545 3_765 ?
Cl1 Cd1 Cl1 83.144(18) . 3_765 ?
Cl1 Cd1 Cl1 96.856(18) 14_665 3_765 ?
Cl1 Cd1 Cl1 83.144(18) 2_645 3_765 ?
Cl1 Cd1 Cl1 83.144(18) 15_545 13_755 ?
Cl1 Cd1 Cl1 180.0 . 13_755 ?
Cl1 Cd1 Cl1 83.144(18) 14_665 13_755 ?
Cl1 Cd1 Cl1 96.856(18) 2_645 13_755 ?
Cl1 Cd1 Cl1 96.856(18) 3_765 13_755 ?
Cl1 Cd1 Cd1 50.015(12) 15_545 4_754 ?
Cl1 Cd1 Cd1 129.985(12) . 4_754 ?
Cl1 Cd1 Cd1 50.015(12) 14_665 4_754 ?
Cl1 Cd1 Cd1 129.985(12) 2_645 4_754 ?
Cl1 Cd1 Cd1 129.985(12) 3_765 4_754 ?
Cl1 Cd1 Cd1 50.015(12) 13_755 4_754 ?
Cl1 Cd1 Cd1 129.985(12) 15_545 4_755 ?
Cl1 Cd1 Cd1 50.015(12) . 4_755 ?
Cl1 Cd1 Cd1 129.985(12) 14_665 4_755 ?
Cl1 Cd1 Cd1 50.015(12) 2_645 4_755 ?
Cl1 Cd1 Cd1 50.015(12) 3_765 4_755 ?
Cl1 Cd1 Cd1 129.985(12) 13_755 4_755 ?
Cd1 Cd1 Cd1 180.0 4_754 4_755 ?
Cd1 Cl1 Cd1 79.97(2) . 4_755 ?
C2 C2 H2A 61.1 16_558 . ?
C2 C2 H2B 61.1 16_558 . ?
H2A C2 H2B 116.3 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.100


# start Validation Reply Form

_vrf_PLAT260_p63mmc              
;
PROBLEM: Large Average Ueq of Residue Including        C2      0.503 Check 
RESPONSE: The quality of crystal is effected by high temperature. 
          Besides, the cations is highly disordered at 363 K.
;

# end Validation Reply Form



_shelx_res_file                  
;

 
TITL P63MMC in P6(3)/mmc
CELL 0.71073   9.5032   9.5032   6.8345  90.000  90.000 120.000
ZERR    2.00   0.0003   0.0003   0.0004   0.000   0.000   0.000
LATT 1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, -X+Y, 0.5+Z
SYMM X-Y, X, 0.5+Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SYMM -Y, -X, 0.5-Z
SYMM -X+Y, Y, 0.5-Z
SYMM X, X-Y, 0.5-Z
SFAC C  H  N  Cl Cd
UNIT 10 28 2 6 2
OMIT 0 54.0
OMIT 0 1 1
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 5
DFIX 1.47 0.0005 N1 C1
DELU 0.02 0.01 C1 C2
DELU 0.02 0.01 N1 C1
SIMU 0.02 0.01 N1 C1
DELU 0.02 0.01 N1 C2
SIMU 0.02 0.01 N1 C2
ISOR N1 C1 C2
WGHT    0.096700    0.108500
FVAR       0.50465
C1    1    0.594170    0.188341    0.875602    10.25000    0.16520    0.15907 =
         0.29299    0.03083    0.01541    0.07953
AFIX   3
H1A   2    0.645830    0.123720    0.870902    10.33370   -1.20000
H1B   2    0.477839    0.123720    0.870902    10.33370   -1.20000
AFIX   0
N1    3    0.666667    0.333333    0.750000    10.08333    0.10922    0.10922 =
         0.24539    0.00000    0.00000    0.05461
CD1   5    1.000000    0.000000    0.000000    10.08333    0.07816    0.07816 =
         0.07832    0.00000    0.00000    0.03908
CL1   4    0.876225    0.123775    0.250000    10.25000    0.11504    0.11504 =
         0.09669    0.00000    0.00000    0.08009
C2    1    0.666667    0.333333    1.120835    10.16667    0.63513    0.63513 =
         0.22746    0.00000    0.00000    0.31756
AFIX   3
H2A   2    0.764830    0.358030    1.188705    10.25000   -1.20000
H2B   2    0.593190    0.358030    1.188705    10.25000   -1.20000
 
HKLF 4
 
REM  P63MMC in P6(3)/mmc
REM R1 =  0.0383 for    216 Fo > 4sig(Fo)  and  0.0423 for all    252 data
REM     18 parameters refined using     26 restraints
 
END  
     
WGHT      0.0718      0.1414 
REM Highest difference peak  0.450,  deepest hole -0.429,  1-sigma level  0.100
Q1    1   0.6667  0.3333  1.0136  10.16667  0.05    0.31
Q2    1   0.7104  0.2896  0.9735  10.50000  0.05    0.27
Q3    1   0.4902  0.1618  0.7500  10.50000  0.05    0.26
Q4    1   0.5215  0.0430  0.7500  10.25000  0.05    0.19
Q5    1   0.9542  0.0458  0.1049  10.50000  0.05    0.18
;
_shelx_res_checksum              83641
