 
data_DMAA_360K
 
_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, C6 H13 N2'
_chemical_formula_sum
 'C6 H13 Cd Cl3 N2' 
_chemical_formula_weight          	331.94

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            62
_space_group_name_H-M_alt         'P n m a'
_space_group_name_Hall            '-P 2ac 2n'
 
_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'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z'
 '-x-1/2, y-1/2, z-1/2'
 
_cell_length_a                    14.7968(9)
_cell_length_b                    6.7636(4)
_cell_length_c                    10.8080(8)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1081.66(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     360(2)
_cell_measurement_reflns_used   2318
_cell_measurement_theta_min     3.3050
_cell_measurement_theta_max     30.3500
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     2.038          
_exptl_crystal_F_000              869
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_absorpt_coefficient_mu     2.711
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.527
_exptl_absorpt_correction_T_max   0.581
_exptl_absorpt_process_details    'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       360(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Rotating-anode X-ray tube' 
_diffrn_measurement_device_type   'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method        ω
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             5151
_diffrn_reflns_av_unetI/netI      0.0159
_diffrn_reflns_av_R_equivalents   0.0176
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.753
_diffrn_reflns_theta_max          30.446
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.802
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.802
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.802
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              1722
_reflns_number_gt                 976
_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 1.171.40.14e (Rigaku OD, 2018)'
_computing_cell_refinement     'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction      'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics      'Bruker SHELXTL' 
_computing_publication_material    'Bruker SHELXTL'
_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)+(0.0762P)²+3.1859P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1422
_refine_ls_number_parameters      74
_refine_ls_number_restraints      53
_refine_ls_R_factor_all           0.0685
_refine_ls_R_factor_gt            0.0480
_refine_ls_wR_factor_ref          0.1677
_refine_ls_wR_factor_gt           0.1533
_refine_ls_goodness_of_fit_ref    1.076
_refine_ls_restrained_S_all       1.100
_refine_ls_shift/su_max           0.002
_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
N2 N 0.3268(11) 0.2500 0.8118(15) 0.258(3) Uani 1 2 d DS TU P . .
H2A H 0.3779 0.2500 0.7668 0.310 Uiso 1 2 d R U P . .
C3 C 0.3630(8) 0.0918(14) 1.0461(14) 0.282(4) Uani 1 1 d D U . . .
H3 H 0.3275 0.0477 1.1175 0.339 Uiso 1 1 d R U . . .
C4 C 0.4390(3) 0.2010(4) 1.0696(8) 0.279(5) Uani 0.5 1 d D U P . .
C1 C 0.2477(12) 0.341(4) 0.7428(16) 0.252(4) Uani 0.5 1 d D U P . .
H1B H 0.2088 0.4546 0.7437 0.379 Uiso 0.5 1 d R U P . .
H1C H 0.3036 0.3743 0.7027 0.379 Uiso 0.5 1 d R U P . .
H1D H 0.2188 0.2493 0.6986 0.379 Uiso 1 2 d R U P . .
N1 N 0.2664(10) 0.2500 0.8641(15) 0.251(3) Uani 1 2 d DS TU P . .
H1A H 0.2153 0.2500 0.9093 0.301 Uiso 1 2 d R U P . .
Cd1 Cd 0.0000 0.0000 1.0000 0.05709(16) Uani 1 2 d S . P . .
Cl2 Cl 0.11504(12) 0.2500 1.10567(18) 0.0689(5) Uani 1 2 d S T P . .
Cl1 Cl 0.01658(12) 0.2500 0.81240(17) 0.0623(4) Uani 1 2 d S T P . .
Cl3 Cl 0.12451(12) -0.2500 0.9279(2) 0.0725(5) Uani 1 2 d S T P . .
C2 C 0.3275(4) 0.0730(6) 0.9002(7) 0.256(3) Uani 1 1 d D U . . .
H2C H 0.3808 0.0110 0.8674 0.307 Uiso 1 1 d R U . . .
H2B H 0.2902 -0.0430 0.9034 0.307 Uiso 1 1 d R U . . .
H4A H 0.4781 0.2499 1.0033 0.307 Uiso 1 2 d DR U P . .
H4B H 0.4683 0.2499 1.1449 0.6(2) Uiso 1 2 d DR . P . .
 
 
_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
N2 N1 1.057(18) . ?
N2 C1 1.518(19) . ?
N2 C1 1.518(19) 7_565 ?
N2 C2 1.532(11) . ?
N2 C2 1.532(11) 7_565 ?
C3 C4 1.368(12) . ?
C3 C2 1.667(16) . ?
C3 C4 1.814(11) 7_565 ?
C4 C4 0.663(6) 7_565 ?
C4 C3 1.814(11) 7_565 ?
C1 C1 1.23(5) 7_565 ?
C1 N1 1.474(19) . ?
N1 C1 1.474(19) 7_565 ?
N1 C2 1.551(11) . ?
N1 C2 1.551(11) 7_565 ?
Cd1 Cl3 2.6191(13) . ?
Cd1 Cl3 2.6192(13) 5_557 ?
Cd1 Cl1 2.6515(14) . ?
Cd1 Cl1 2.6515(14) 5_557 ?
Cd1 Cl2 2.6572(13) 5_557 ?
Cd1 Cl2 2.6573(13) . ?
Cd1 Cd1 3.3818(2) 3_557 ?
Cd1 Cd1 3.3818(2) 3_547 ?
Cl2 Cd1 2.6573(13) 3_557 ?
Cl1 Cd1 2.6515(14) 3_557 ?
Cl3 Cd1 2.6191(13) 3_547 ?
 
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 N2 C1 67.1(12) . . ?
N1 N2 C1 67.1(12) . 7_565 ?
C1 N2 C1 48(2) . 7_565 ?
N1 N2 C2 70.9(9) . . ?
C1 N2 C2 129.0(13) . . ?
C1 N2 C2 89.7(11) 7_565 . ?
N1 N2 C2 70.9(9) . 7_565 ?
C1 N2 C2 89.7(11) . 7_565 ?
C1 N2 C2 129.0(13) 7_565 7_565 ?
C2 N2 C2 102.8(11) . 7_565 ?
C4 C3 C2 118.4(10) . . ?
C4 C3 C4 17.9(2) . 7_565 ?
C2 C3 C4 112.7(8) . 7_565 ?
C4 C4 C3 122.7(4) 7_565 . ?
C4 C4 C3 39.4(4) 7_565 7_565 ?
C3 C4 C3 83.2(7) . 7_565 ?
C1 C1 N1 65.3(11) 7_565 . ?
C1 C1 N2 66.1(10) 7_565 . ?
N1 C1 N2 41.3(9) . . ?
N2 N1 C1 71.5(11) . . ?
N2 N1 C1 71.5(11) . 7_565 ?
C1 N1 C1 49(2) . 7_565 ?
N2 N1 C2 69.0(9) . . ?
C1 N1 C2 131.0(13) . . ?
C1 N1 C2 90.6(11) 7_565 . ?
N2 N1 C2 69.0(9) . 7_565 ?
C1 N1 C2 90.6(11) . 7_565 ?
C1 N1 C2 131.0(13) 7_565 7_565 ?
C2 N1 C2 101.1(10) . 7_565 ?
Cl3 Cd1 Cl3 180.00(5) . 5_557 ?
Cl3 Cd1 Cl1 96.85(5) . . ?
Cl3 Cd1 Cl1 83.15(5) 5_557 . ?
Cl3 Cd1 Cl1 83.15(5) . 5_557 ?
Cl3 Cd1 Cl1 96.85(5) 5_557 5_557 ?
Cl1 Cd1 Cl1 180.0 . 5_557 ?
Cl3 Cd1 Cl2 84.95(5) . 5_557 ?
Cl3 Cd1 Cl2 95.05(5) 5_557 5_557 ?
Cl1 Cd1 Cl2 97.84(5) . 5_557 ?
Cl1 Cd1 Cl2 82.16(5) 5_557 5_557 ?
Cl3 Cd1 Cl2 95.05(5) . . ?
Cl3 Cd1 Cl2 84.95(5) 5_557 . ?
Cl1 Cd1 Cl2 82.16(5) . . ?
Cl1 Cd1 Cl2 97.84(5) 5_557 . ?
Cl2 Cd1 Cl2 180.0 5_557 . ?
Cl3 Cd1 Cd1 130.21(3) . 3_557 ?
Cl3 Cd1 Cd1 49.79(3) 5_557 3_557 ?
Cl1 Cd1 Cd1 50.38(3) . 3_557 ?
Cl1 Cd1 Cd1 129.62(3) 5_557 3_557 ?
Cl2 Cd1 Cd1 129.52(2) 5_557 3_557 ?
Cl2 Cd1 Cd1 50.48(2) . 3_557 ?
Cl3 Cd1 Cd1 49.79(3) . 3_547 ?
Cl3 Cd1 Cd1 130.21(3) 5_557 3_547 ?
Cl1 Cd1 Cd1 129.62(3) . 3_547 ?
Cl1 Cd1 Cd1 50.38(3) 5_557 3_547 ?
Cl2 Cd1 Cd1 50.48(2) 5_557 3_547 ?
Cl2 Cd1 Cd1 129.52(2) . 3_547 ?
Cd1 Cd1 Cd1 180.0 3_557 3_547 ?
Cd1 Cl2 Cd1 79.04(5) . 3_557 ?
Cd1 Cl1 Cd1 79.24(5) 3_557 . ?
Cd1 Cl3 Cd1 80.42(5) 3_547 . ?
N2 C2 N1 40.1(7) . . ?
N2 C2 C3 122.2(7) . . ?
N1 C2 C3 111.3(8) . . ?
 
_refine_diff_density_max    0.575
_refine_diff_density_min   -0.777
_refine_diff_density_rms    0.137




