# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1550866'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cd2 Cl8, 4(C2 Cl N)'
_chemical_formula_sum            'C8 Cd2 Cl12 N4'
_chemical_formula_weight         802.34

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           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_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, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   7.5041(15)
_cell_length_b                   24.658(5)
_cell_length_c                   7.4996(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1387.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    863
_cell_measurement_theta_min      3.179
_cell_measurement_theta_max      27.482

_exptl_crystal_description       flake
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.690
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4530
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.179
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             863
_reflns_number_gt                656
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.1381P)²+15.1768P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         863
_refine_ls_number_parameters     48
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.2258
_refine_ls_wR_factor_gt          0.2072
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.059
_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
C2 C 0.5000 0.296(2) 0.408(9) 0.29(3) Uani 0.5 2 d DS TU P . .
C2A C 0.5000 0.3141(17) 0.474(11) 0.29(3) Uani 0.5 2 d DS TU P . .
C1 C 0.5000 0.3481(19) 0.516(7) 0.156(18) Uani 0.5 2 d DS TU P . .
C1A C 0.5000 0.3618(18) 0.594(6) 0.156(18) Uani 0.5 2 d DS TU P . .
Cl3 Cl 0.5000 0.2560(16) 0.608(9) 0.47(2) Uani 0.5 2 d DS TU P . .
Cl3A Cl 0.5000 0.2420(17) 0.506(9) 0.47(2) Uani 0.5 2 d DS TU P . .
N1 N 0.5000 0.407(2) 0.461(11) 0.080(13) Uani 0.5 2 d DS TU P . .
N1A N 0.5000 0.410(3) 0.503(11) 0.080(13) Uani 0.5 2 d S TU P . .
Cd1 Cd 0.5000 0.5000 0.0000 0.0346(5) Uani 1 4 d S TU P . .
Cl1 Cl 0.7500 0.50923(18) 0.2500 0.0714(12) Uani 1 2 d S TU P . .
Cl2 Cl 0.5000 0.39850(18) 0.0399(6) 0.0925(19) Uani 1 2 d S TU P . .

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
C2 0.40(7) 0.101(12) 0.37(4) -0.032(19) 0.000 0.000
C2A 0.40(7) 0.101(12) 0.37(4) -0.032(19) 0.000 0.000
C1 0.22(4) 0.138(14) 0.11(3) 0.030(16) 0.000 0.000
C1A 0.22(4) 0.138(14) 0.11(3) 0.030(16) 0.000 0.000
Cl3 0.83(5) 0.125(13) 0.46(6) 0.040(19) 0.000 0.000
Cl3A 0.83(5) 0.125(13) 0.46(6) 0.040(19) 0.000 0.000
N1 0.106(15) 0.097(11) 0.04(4) -0.020(15) 0.000 0.000
N1A 0.106(15) 0.097(11) 0.04(4) -0.020(15) 0.000 0.000
Cd1 0.0264(7) 0.0511(8) 0.0264(7) 0.0011(4) 0.000 0.000
Cl1 0.0394(17) 0.135(4) 0.0400(17) 0.000 -0.0160(16) 0.000
Cl2 0.160(6) 0.0499(19) 0.067(2) 0.0019(18) 0.000 0.000

_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
C2 C1 1.52(2) . ?
C2 Cl3 1.79(2) . ?
C2A C1A 1.48(2) . ?
C2A Cl3A 1.79(2) . ?
C1 N1 1.51(2) . ?
C1A N1A 1.36(8) . ?
Cd1 Cl2 2.520(4) . ?
Cd1 Cl2 2.521(4) 9_665 ?
Cd1 Cl1 2.6620(5) 9_665 ?
Cd1 Cl1 2.6620(5) 14_456 ?
Cd1 Cl1 2.6620(5) 6_654 ?
Cd1 Cl1 2.6621(5) . ?
Cl1 Cd1 2.6621(5) 6_655 ?

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
C1 C2 Cl3 91(3) . . ?
C1A C2A Cl3A 135(6) . . ?
N1 C1 C2 132(6) . . ?
N1A C1A C2A 113(6) . . ?
Cl2 Cd1 Cl2 180.0 . 9_665 ?
Cl2 Cd1 Cl1 89.92(12) . 9_665 ?
Cl2 Cd1 Cl1 90.08(12) 9_665 9_665 ?
Cl2 Cd1 Cl1 90.08(12) . 14_456 ?
Cl2 Cd1 Cl1 89.92(12) 9_665 14_456 ?
Cl1 Cd1 Cl1 90.38(2) 9_665 14_456 ?
Cl2 Cd1 Cl1 89.92(12) . 6_654 ?
Cl2 Cd1 Cl1 90.08(12) 9_665 6_654 ?
Cl1 Cd1 Cl1 89.62(2) 9_665 6_654 ?
Cl1 Cd1 Cl1 180.0 14_456 6_654 ?
Cl2 Cd1 Cl1 90.08(12) . . ?
Cl2 Cd1 Cl1 89.92(12) 9_665 . ?
Cl1 Cd1 Cl1 180.0 9_665 . ?
Cl1 Cd1 Cl1 89.62(2) 14_456 . ?
Cl1 Cd1 Cl1 90.38(2) 6_654 . ?
Cd1 Cl1 Cd1 170.19(19) . 6_655 ?

_refine_diff_density_max         1.921
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.247

_shelx_res_file                  
;

    2.res created by SHELXL-2014/7

TITL 2 in Cmca
CELL 0.71073   7.5041  24.6579   7.4996  90.000  90.000  90.000
ZERR   14.00   0.0015   0.0049   0.0015   0.000   0.000   0.000
LATT 7
SYMM -X, 0.5-Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM X, -Y, -Z
SFAC C  H  N  Cl Cd
UNIT 16 0 8 24 4
L.S. 50
ACTA
BOND
FMAP 2
PLAN 20
delu
dfix 1.8 c2 cl3
dfix 1.5 c1 c2
dfix 1.5 c1 n1
dfix 1.8 c2a cl3a
dfix 1.5 c1a c2a
dfix 1.5 c1a n1
eadp c1 c1a
eadp c2 c2a
eadp n1 n1a
eadp cl3 cl3a
isor c1 c1a c2 c2a n1 n1a cl3 cl3a
FREE N1   N1A
FREE C1A  N1
FREE C1   N1A
FREE C1A  Cl3
FREE C1   Cl3
FREE C2A  Cl3
FREE C2   Cl3A
FREE Cl3  Cl3A
FREE C2A  C1
FREE C1   C1A
FREE C2   C2A
WGHT    0.138100   15.176800
FVAR       0.20387
MOLE 1
C2    1    0.500000    0.295725    0.408310    10.25000    0.40078    0.10138 =
         0.36805   -0.03181    0.00000    0.00000
C2A   1    0.500000    0.314132    0.474499    10.25000    0.40078    0.10138 =
         0.36805   -0.03181    0.00000    0.00000
C1    1    0.500000    0.348092    0.516047    10.25000    0.22071    0.13776 =
         0.11017    0.02987    0.00000    0.00000
C1A   1    0.500000    0.361771    0.593796    10.25000    0.22071    0.13776 =
         0.11017    0.02987    0.00000    0.00000
CL3   4    0.500000    0.256036    0.608360    10.25000    0.82687    0.12536 =
         0.45647    0.03988    0.00000    0.00000
CL3A  4    0.500000    0.241958    0.505642    10.25000    0.82687    0.12536 =
         0.45647    0.03988    0.00000    0.00000
N1    3    0.500000    0.406910    0.461001    10.25000    0.10618    0.09731 =
         0.03756   -0.01955    0.00000    0.00000
N1A   3    0.500000    0.409591    0.503316    10.25000    0.10618    0.09731 =
         0.03756   -0.01955    0.00000    0.00000
CD1   5    0.500000    0.500000    0.000000    10.25000    0.02636    0.05105 =
         0.02642    0.00110    0.00000    0.00000
CL1   4    0.750000    0.509231    0.250000    10.50000    0.03938    0.13481 =
         0.04002    0.00000   -0.01602    0.00000
CL2   4    0.500000    0.398505    0.039866    10.50000    0.16011    0.04989 =
         0.06736    0.00187    0.00000    0.00000
HKLF 4

REM  2 in Cmca
REM R1 =  0.0740 for     656 Fo > 4sig(Fo)  and  0.0943 for all     863 data
REM     48 parameters refined using     67 restraints

END

WGHT      0.1431     12.6886

REM Highest difference peak  1.921,  deepest hole -1.067,  1-sigma level  0.247
Q1    1   0.4279  0.3998 -0.0089  11.00000  0.05    1.92
Q2    1   0.6201  0.2890  0.3668  11.00000  0.05    0.99
Q3    1   0.6509  0.2892  0.5843  11.00000  0.05    0.94
Q4    1   0.7500  0.4737  0.2500  10.50000  0.05    0.89
Q5    1   0.5790  0.3612  0.5152  11.00000  0.05    0.84
Q6    1   0.5000  0.5400 -0.0017  10.50000  0.05    0.84
Q7    1   0.5783  0.3168  0.5748  11.00000  0.05    0.77
Q8    1   0.7500  0.5250  0.2500  10.50000  0.05    0.71
Q9    1   0.5000  0.3523  0.7523  10.50000  0.05    0.23
Q10   1   0.2972  0.3891 -0.0238  11.00000  0.05    0.22
Q11   1   0.2996  0.4060 -0.0247  11.00000  0.05    0.21
Q12   1   0.4496  0.3336  0.0059  11.00000  0.05    0.18
Q13   1   0.3534  0.3602 -0.0236  11.00000  0.05    0.18
Q14   1   1.0000  0.5078  0.1142  10.50000  0.05    0.17
Q15   1   0.4129  0.4824  0.0510  11.00000  0.05    0.16
Q16   1   0.3546  0.4425  0.0104  11.00000  0.05    0.16
Q17   1   0.4292  0.3547 -0.0909  11.00000  0.05    0.16
Q18   1   0.5000  0.4935  0.1468  10.50000  0.05    0.16
Q19   1   0.7097  0.3963  0.6076  11.00000  0.05    0.15
Q20   1   0.4246  0.3177  0.7681  11.00000  0.05    0.14
;
_shelx_res_checksum              74326
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1550869'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H14 Br4 Cd Cl2 N2'
_chemical_formula_sum            'C4 H14 Br4 Cd Cl2 N2'
_chemical_formula_weight         593.11

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'
Br Br -0.2901 2.4595 '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           orthorhombic
_symmetry_space_group_name_H-M   'A b a 2 '

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

_cell_length_a                   7.9926(16)
_cell_length_b                   24.108(5)
_cell_length_c                   7.9560(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1533.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1358
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      24.99

_exptl_crystal_description       flake
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    12.167
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5788
_diffrn_reflns_av_R_equivalents  0.1143
_diffrn_reflns_av_sigmaI/netI    0.1244
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1358
_reflns_number_gt                815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0891P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1358
_refine_ls_number_parameters     85
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2076
_refine_ls_wR_factor_gt          0.1846
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      0.976
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.990(2) 0.6518(5) 0.883(3) 0.130(2) Uani 0.50 1 d PDU A 1
H1A H 1.0248 0.6511 0.7661 0.155 Uiso 0.50 1 calc PR A 1
H1B H 0.8691 0.6510 0.8841 0.155 Uiso 0.50 1 calc PR A 1
C2 C 1.046(2) 0.7081(7) 0.957(3) 0.131(4) Uani 0.50 1 d PDU A 1
H2A H 1.1540 0.7199 0.9151 0.158 Uiso 0.50 1 calc PR A 1
H2B H 1.0456 0.7082 1.0787 0.158 Uiso 0.50 1 calc PR A 1
Cl1 Cl 0.8753(17) 0.7486(5) 0.869(2) 0.255(6) Uani 0.50 1 d PDU A 1
N1 N 1.049(2) 0.6000(7) 0.961(3) 0.130(2) Uani 0.50 1 d PDU A 1
H1C H 1.0426 0.5725 0.8866 0.194 Uiso 0.50 1 calc PR A 1
H1D H 0.9855 0.5921 1.0496 0.194 Uiso 0.50 1 calc PR A 1
H1E H 1.1549 0.6041 0.9939 0.194 Uiso 0.50 1 calc PR A 1
C1' C 0.984(2) 0.6459(8) 0.8055(19) 0.141(3) Uani 0.50 1 d PDU B 2
H1'A H 1.0692 0.6742 0.7901 0.169 Uiso 0.50 1 calc PR B 2
H1'B H 0.9341 0.6319 0.7028 0.169 Uiso 0.50 1 calc PR B 2
C2' C 0.877(3) 0.6485(8) 0.961(3) 0.140(3) Uani 0.50 1 d PDU B 2
H2'A H 0.9058 0.6199 1.0419 0.168 Uiso 0.50 1 calc PR B 2
H2'B H 0.7586 0.6469 0.9354 0.168 Uiso 0.50 1 calc PR B 2
Cl1' Cl 0.944(2) 0.7178(5) 1.0300(19) 0.219(5) Uani 0.50 1 d PDU B 2
N1' N 1.003(2) 0.6072(9) 0.948(3) 0.130(2) Uani 0.50 1 d PDU B 2
H1'C H 1.0594 0.5774 0.9155 0.194 Uiso 0.50 1 calc PR B 2
H1'D H 0.9019 0.5971 0.9847 0.194 Uiso 0.50 1 calc PR B 2
H1'E H 1.0578 0.6240 1.0313 0.194 Uiso 0.50 1 calc PR B 2
Cd1 Cd 0.0000 0.5000 0.4138(3) 0.0832(3) Uani 1 2 d SU . .
Br2 Br 0.2395(2) 0.48916(6) 0.664810(18) 0.0832(3) Uani 1 1 d U . .
Br1 Br 0.04554(18) 0.60812(7) 0.4261(5) 0.1373(8) Uani 1 1 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
C1 0.145(5) 0.100(2) 0.145(5) 0.066(3) 0.045(5) -0.060(3)
C2 0.149(6) 0.094(3) 0.151(11) 0.047(5) 0.043(6) -0.022(5)
Cl1 0.245(7) 0.198(4) 0.322(16) 0.006(10) -0.021(8) 0.092(5)
N1 0.145(5) 0.100(2) 0.145(5) 0.066(3) 0.045(5) -0.060(3)
C1' 0.148(8) 0.129(6) 0.146(4) 0.069(3) 0.016(4) -0.039(9)
C2' 0.130(6) 0.137(4) 0.154(6) 0.081(6) 0.018(5) -0.045(4)
Cl1' 0.275(12) 0.135(5) 0.247(8) 0.018(4) 0.023(9) -0.015(7)
N1' 0.145(5) 0.100(2) 0.145(5) 0.066(3) 0.045(5) -0.060(3)
Cd1 0.0547(5) 0.1317(8) 0.0633(5) 0.000 0.000 -0.0078(5)
Br2 0.0547(5) 0.1317(8) 0.0633(5) 0.000 0.000 -0.0078(5)
Br1 0.0825(8) 0.0776(10) 0.252(2) 0.0498(17) -0.0361(16) -0.0099(8)

_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 C2 1.54(2) . ?
C1 N1 1.47(2) . ?
C2 Cl1 1.81(2) . ?
C1' C2' 1.51(2) . ?
C1' N1' 1.48(2) . ?
C2' Cl1' 1.84(2) . ?
Cd1 Br1 2.6337(18) 2_565 ?
Cd1 Br1 2.6337(18) . ?
Cd1 Br2 2.779(2) . ?
Cd1 Br2 2.779(2) 2_565 ?
Cd1 Br2 2.886(2) 7_454 ?
Cd1 Br2 2.886(2) 8_544 ?
Br2 Cd1 2.886(2) 7 ?

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
C2 C1 N1 119.7(19) . . ?
C1 C2 Cl1 96.5(14) . . ?
C2' C1' N1' 56.6(13) . . ?
C1' C2' Cl1' 96.8(14) . . ?
Br1 Cd1 Br1 175.7(2) 2_565 . ?
Br1 Cd1 Br2 88.59(9) 2_565 . ?
Br1 Cd1 Br2 88.35(9) . . ?
Br1 Cd1 Br2 88.35(9) 2_565 2_565 ?
Br1 Cd1 Br2 88.59(9) . 2_565 ?
Br2 Cd1 Br2 88.12(9) . 2_565 ?
Br1 Cd1 Br2 90.88(8) 2_565 7_454 ?
Br1 Cd1 Br2 92.04(8) . 7_454 ?
Br2 Cd1 Br2 177.38(9) . 7_454 ?
Br2 Cd1 Br2 89.301(17) 2_565 7_454 ?
Br1 Cd1 Br2 92.04(8) 2_565 8_544 ?
Br1 Cd1 Br2 90.88(8) . 8_544 ?
Br2 Cd1 Br2 89.301(17) . 8_544 ?
Br2 Cd1 Br2 177.38(9) 2_565 8_544 ?
Br2 Cd1 Br2 93.29(9) 7_454 8_544 ?
Cd1 Br2 Cd1 169.09(6) . 7 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.320
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.184
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1550868'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br Cd Cl3, 3(C H3.50 Cl0.50 N0.50)'
_chemical_formula_sum            'C4 H14 Br Cd Cl5 N2'
_chemical_formula_weight         459.73

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'
Br Br -0.2901 2.4595 '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           orthorhombic
_symmetry_space_group_name_H-M   'A b a 2 '


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

_cell_length_a                   7.6707(10)
_cell_length_b                   24.6215(19)
_cell_length_c                   7.5742(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1430.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1508
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      27.47

_exptl_crystal_description       flake
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    5.219
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4104
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1508
_reflns_number_gt                1089
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0648P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1508
_refine_ls_number_parameters     106
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1389
_refine_ls_wR_factor_gt          0.1266
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.008

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
C2 C 0.472(3) 0.6845(9) 0.483(4) 0.125(7) Uani 0.50 1 d PU A 1
H2A H 0.3624 0.6808 0.5457 0.150 Uiso 0.50 1 calc PR A 1
H2B H 0.4448 0.6855 0.3579 0.150 Uiso 0.50 1 calc PR A 1
C1 C 0.563(3) 0.6408(7) 0.513(4) 0.091(6) Uani 0.50 1 d PU A 1
H1A H 0.6534 0.6503 0.5968 0.109 Uiso 0.50 1 calc PR A 1
H1B H 0.6216 0.6314 0.4030 0.109 Uiso 0.50 1 calc PR A 1
Cl3 Cl 0.5671(13) 0.7512(3) 0.543(3) 0.187(4) Uani 0.50 1 d PU A 1
N1 N 0.4763(18) 0.5903(5) 0.579(3) 0.056(6) Uani 0.50 1 d PU A 1
H1C H 0.5566 0.5650 0.6004 0.083 Uiso 0.50 1 calc PR A 1
H1D H 0.4019 0.5781 0.4980 0.083 Uiso 0.50 1 calc PR A 1
H1E H 0.4189 0.5978 0.6782 0.083 Uiso 0.50 1 calc PR A 1
C2A C 0.608(4) 0.6787(12) 0.477(4) 0.146(7) Uani 0.50 1 d PU B 2
H2'A H 0.6292 0.6947 0.3616 0.175 Uiso 0.50 1 calc PR B 2
H2'B H 0.7136 0.6626 0.5230 0.175 Uiso 0.50 1 calc PR B 2
C1A C 0.499(4) 0.6515(15) 0.477(6) 0.135(7) Uani 0.50 1 d PU B 2
H1'A H 0.4651 0.6473 0.3550 0.162 Uiso 0.50 1 calc PR B 2
H1'B H 0.4051 0.6708 0.5350 0.162 Uiso 0.50 1 calc PR B 2
Cl3A Cl 0.505(2) 0.7260(7) 0.631(2) 0.279(8) Uani 0.50 1 d PU B 2
N1A N 0.499(3) 0.5998(12) 0.549(5) 0.115(8) Uani 0.50 1 d PU B 2
H1'C H 0.3975 0.5837 0.5242 0.172 Uiso 0.50 1 calc PR B 2
H1'D H 0.5120 0.6019 0.6652 0.172 Uiso 0.50 1 calc PR B 2
H1'E H 0.5855 0.5806 0.5025 0.172 Uiso 0.50 1 calc PR B 2
Cd1 Cd 0.5000 0.5000 1.0404 0.0441(2) Uani 1 2 d SU . .
Cl2 Cl 0.5607(7) 0.3916(2) 1.0597(19) 0.075(2) Uani 0.50 1 d PU . .
Br1 Br 0.4645(4) 0.60306(12) 1.0274(9) 0.0846(13) Uani 0.50 1 d PU . .
Cl1 Cl 0.7469(11) 0.51243(7) 0.7886(7) 0.0578(5) Uani 1 1 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
C2 0.209(15) 0.035(6) 0.131(15) 0.040(8) -0.021(13) -0.019(8)
C1 0.126(13) 0.055(6) 0.091(15) 0.040(9) -0.003(12) -0.026(7)
Cl3 0.265(8) 0.076(4) 0.220(9) 0.010(14) -0.017(15) -0.076(4)
N1 0.049(8) 0.033(6) 0.085(16) 0.030(8) -0.002(8) -0.005(5)
C2A 0.189(14) 0.112(11) 0.136(15) 0.019(9) -0.021(14) -0.004(10)
C1A 0.187(16) 0.113(8) 0.106(15) 0.050(7) -0.024(14) -0.003(11)
Cl3A 0.421(19) 0.179(9) 0.237(16) -0.044(10) 0.057(10) 0.020(11)
N1A 0.129(18) 0.132(8) 0.083(14) 0.068(11) -0.030(17) 0.028(11)
Cd1 0.0402(4) 0.0498(4) 0.0422(3) 0.000 0.000 0.0024(2)
Cl2 0.038(2) 0.047(3) 0.141(6) 0.018(5) -0.037(4) 0.0045(19)
Br1 0.0878(19) 0.0416(11) 0.124(3) -0.007(2) -0.041(2) 0.0126(11)
Cl1 0.0346(9) 0.1001(12) 0.0388(8) 0.006(3) 0.0153(6) 0.003(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
C2 C1 1.30(3) . ?
C2 Cl3 1.85(2) . ?
C1 N1 1.50(2) . ?
C2A C1A 1.07(4) . ?
C2A Cl3A 1.83(3) . ?
C1A N1A 1.38(4) . ?
C1A Cl3A 2.17(4) . ?
Cd1 Br1 2.554(3) . ?
Cd1 Br1 2.554(3) 2_665 ?
Cd1 Cl2 2.714(6) 2_665 ?
Cd1 Cl2 2.714(6) . ?
Cd1 Cl1 2.705(6) 2_665 ?
Cd1 Cl1 2.705(6) . ?
Cd1 Cl1 2.720(6) 8_645 ?
Cd1 Cl1 2.720(6) 7_455 ?
Cl2 Br1 0.339(13) 2_665 ?
Br1 Cl2 0.339(13) 2_665 ?
Cl1 Cd1 2.720(6) 7_554 ?

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
C1 C2 Cl3 119(2) . . ?
C2 C1 N1 120(2) . . ?
C1A C2A Cl3A 94(4) . . ?
C2A C1A N1A 126(4) . . ?
C2A C1A Cl3A 57(3) . . ?
N1A C1A Cl3A 125(3) . . ?
C2A Cl3A C1A 29.4(13) . . ?
Br1 Cd1 Br1 175.6(3) . 2_665 ?
Br1 Cd1 Cl2 6.5(3) . 2_665 ?
Br1 Cd1 Cl2 176.12(19) 2_665 2_665 ?
Br1 Cd1 Cl2 176.12(19) . . ?
Br1 Cd1 Cl2 6.5(3) 2_665 . ?
Cl2 Cd1 Cl2 173.8(6) 2_665 . ?
Br1 Cd1 Cl1 90.61(11) . 2_665 ?
Br1 Cd1 Cl1 86.27(13) 2_665 2_665 ?
Cl2 Cd1 Cl1 91.7(2) 2_665 2_665 ?
Cl2 Cd1 Cl1 92.7(2) . 2_665 ?
Br1 Cd1 Cl1 86.27(13) . . ?
Br1 Cd1 Cl1 90.61(11) 2_665 . ?
Cl2 Cd1 Cl1 92.7(2) 2_665 . ?
Cl2 Cd1 Cl1 91.7(2) . . ?
Cl1 Cd1 Cl1 90.3(3) 2_665 . ?
Br1 Cd1 Cl1 89.48(11) . 8_645 ?
Br1 Cd1 Cl1 93.58(13) 2_665 8_645 ?
Cl2 Cd1 Cl1 88.6(2) 2_665 8_645 ?
Cl2 Cd1 Cl1 87.2(2) . 8_645 ?
Cl1 Cd1 Cl1 178.9(3) 2_665 8_645 ?
Cl1 Cd1 Cl1 88.557(13) . 8_645 ?
Br1 Cd1 Cl1 93.58(13) . 7_455 ?
Br1 Cd1 Cl1 89.48(11) 2_665 7_455 ?
Cl2 Cd1 Cl1 87.2(2) 2_665 7_455 ?
Cl2 Cd1 Cl1 88.6(2) . 7_455 ?
Cl1 Cd1 Cl1 88.557(13) 2_665 7_455 ?
Cl1 Cd1 Cl1 178.9(3) . 7_455 ?
Cl1 Cd1 Cl1 92.6(3) 8_645 7_455 ?
Br1 Cl2 Cd1 58.7(15) 2_665 . ?
Cl2 Br1 Cd1 114.8(17) 2_665 . ?
Cd1 Cl1 Cd1 166.99(7) . 7_554 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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_2_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1550867'
_audit_update_record             
;
2017-05-18 deposited with the CCDC.
2018-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H14 Br Cd Cl5 N2'
_chemical_formula_sum            'C4 H14 Br Cd Cl5 N2'
_chemical_formula_weight         459.73

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'
Br Br -0.2901 2.4595 '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           orthorhombic
_symmetry_space_group_name_H-M   'A b a 2 '

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

_cell_length_a                   7.649(11)
_cell_length_b                   24.42(4)
_cell_length_c                   7.579(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1416(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1249
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.44

_exptl_crystal_description       flake
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_absorpt_coefficient_mu    5.274
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3996
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         24.98
_reflns_number_total             1174
_reflns_number_gt                932
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.2000P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.36(10)
_refine_ls_number_reflns         1174
_refine_ls_number_parameters     52
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.2938
_refine_ls_wR_factor_gt          0.2524
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.183
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.5000 0.51488(14) 0.04053(15) Uani 1 2 d SU . .
Cl1 Cl 0.2574(4) 0.48834(7) 0.2603(2) 0.0701(5) Uani 1 1 d U . .
Cl2 Cl 0.0174(5) 0.60741(18) 0.4695(5) 0.0690(11) Uani 0.50 1 d PU . .
Br1 Br 0.05055(16) 0.60489(5) 0.5364(3) 0.0652(4) Uani 0.50 1 d PU . .
N1 N -0.0063(8) 0.40400(6) 1.0021(6) 0.333(3) Uani 1 1 d DU . .
H1C H -0.1079 0.4091 0.9417 0.499 Uiso 1 1 calc R . .
H1D H 0.0855 0.4057 0.9260 0.499 Uiso 1 1 calc R . .
H1E H 0.0050 0.4306 1.0854 0.499 Uiso 1 1 calc R . .
Cl3 Cl 0.0470(7) 0.25401(18) 1.0557(10) 0.333(3) Uani 1 1 d DU . .
C2 C 0.0789(5) 0.31501(8) 0.9512(4) 0.333(3) Uani 1 1 d DU . .
H1A H 0.2009 0.3277 0.9667 0.399 Uiso 1 1 d R . .
H1B H 0.0399 0.3163 0.8268 0.399 Uiso 1 1 d R . .
C1 C -0.0090(6) 0.34899(9) 1.0899(3) 0.333(3) Uani 1 1 d DU . .
H2A H 0.0297 0.3418 1.2124 0.399 Uiso 1 1 d R . .
H2B H -0.1272 0.3335 1.0714 0.399 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 0.0354(2) 0.0546(3) 0.0316(3) 0.000 0.000 -0.00433(17)
Cl1 0.0265(6) 0.1604(14) 0.0235(6) -0.0051(13) 0.0135(5) 0.0076(12)
Cl2 0.079(2) 0.0580(16) 0.070(2) 0.0076(15) -0.0373(12) 0.0062(13)
Br1 0.0534(5) 0.0496(6) 0.0926(8) 0.0033(9) -0.0365(8) -0.0001(5)
N1 0.328(5) 0.227(3) 0.442(6) 0.219(3) -0.113(5) -0.027(4)
Cl3 0.328(5) 0.227(3) 0.442(6) 0.219(3) -0.113(5) -0.027(4)
C2 0.328(5) 0.227(3) 0.442(6) 0.219(3) -0.113(5) -0.027(4)
C1 0.328(5) 0.227(3) 0.442(6) 0.219(3) -0.113(5) -0.027(4)

_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 Br1 2.595(4) . ?
Cd1 Br1 2.595(4) 2_565 ?
Cd1 Cl2 2.649(6) . ?
Cd1 Cl2 2.649(6) 2_565 ?
Cd1 Cl1 2.643(3) 8_545 ?
Cd1 Cl1 2.643(3) 7_455 ?
Cd1 Cl1 2.771(4) 2_565 ?
Cd1 Cl1 2.771(4) . ?
Cl1 Cd1 2.643(3) 7_554 ?
Cl2 Br1 0.570(4) . ?
N1 C1 1.499(3) . ?
Cl3 C2 1.704(6) . ?
C2 C1 1.499(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
_geom_angle_publ_flag
Br1 Cd1 Br1 172.81(11) . 2_565 ?
Br1 Cd1 Cl2 12.43(9) . . ?
Br1 Cd1 Cl2 173.15(10) 2_565 . ?
Br1 Cd1 Cl2 173.15(10) . 2_565 ?
Br1 Cd1 Cl2 12.43(9) 2_565 2_565 ?
Cl2 Cd1 Cl2 165.07(17) . 2_565 ?
Br1 Cd1 Cl1 87.57(6) . 8_545 ?
Br1 Cd1 Cl1 87.37(6) 2_565 8_545 ?
Cl2 Cd1 Cl1 99.37(9) . 8_545 ?
Cl2 Cd1 Cl1 91.15(10) 2_565 8_545 ?
Br1 Cd1 Cl1 87.37(6) . 7_455 ?
Br1 Cd1 Cl1 87.56(6) 2_565 7_455 ?
Cl2 Cd1 Cl1 91.15(10) . 7_455 ?
Cl2 Cd1 Cl1 99.37(9) 2_565 7_455 ?
Cl1 Cd1 Cl1 90.52(15) 8_545 7_455 ?
Br1 Cd1 Cl1 92.76(6) . 2_565 ?
Br1 Cd1 Cl1 92.25(6) 2_565 2_565 ?
Cl2 Cd1 Cl1 81.00(9) . 2_565 ?
Cl2 Cd1 Cl1 88.60(10) 2_565 2_565 ?
Cl1 Cd1 Cl1 179.29(10) 8_545 2_565 ?
Cl1 Cd1 Cl1 88.86(11) 7_455 2_565 ?
Br1 Cd1 Cl1 92.25(6) . . ?
Br1 Cd1 Cl1 92.76(6) 2_565 . ?
Cl2 Cd1 Cl1 88.60(10) . . ?
Cl2 Cd1 Cl1 81.00(9) 2_565 . ?
Cl1 Cd1 Cl1 88.86(11) 8_545 . ?
Cl1 Cd1 Cl1 179.29(10) 7_455 . ?
Cl1 Cd1 Cl1 91.75(15) 2_565 . ?
Cd1 Cl1 Cd1 167.91(8) 7_554 . ?
Br1 Cl2 Cd1 78.5(4) . . ?
Cl2 Br1 Cd1 89.1(5) . . ?
C1 C2 Cl3 95.4(3) . . ?
C2 C1 N1 100.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         4.498
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.302
