data_(Me)2NEt_93K _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, C4 H12 N" _chemical_formula_sum 'C4 H12 Cd Cl3 N' _chemical_formula_weight 292.91 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7388(3) _cell_length_b 15.1099(7) _cell_length_c 10.4269(7) _cell_angle_alpha 90 _cell_angle_beta 118.749(4) _cell_angle_gamma 90 _cell_volume 930.82(9) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3658 _cell_measurement_theta_min 2.5980 _cell_measurement_theta_max 31.4620 _exptl_crystal_description rodlike _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 2.090 _exptl_crystal_F_000 568 _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 3.131 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_process_details 'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 93(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 \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7890 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.604 _diffrn_reflns_theta_max 31.489 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.815 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.815 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.815 _diffrn_reflns_point_group_measured_fraction_full 0.981 _reflns_number_total 2517 _reflns_number_gt 1925 _reflns_threshold_expression 'I > 2\s(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/[\s^2^(Fo^2^)+56.7716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2517 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 1.0000 1.0000 0.5000 0.01261(13) Uani 1 2 d S . P . . Cd2 Cd 0.5000 1.0000 0.5000 0.01259(13) Uani 1 2 d S . P . . Cl1 Cl 0.6527(3) 1.10206(11) 0.35829(16) 0.0167(3) Uani 1 1 d . . . . . Cl2 Cl 0.9175(2) 1.02521(10) 0.72313(16) 0.0138(3) Uani 1 1 d . . . . . Cl3 Cl 0.6956(3) 0.87346(11) 0.43604(17) 0.0166(3) Uani 1 1 d . . . . . N1 N 0.8876(12) 0.1590(5) 0.1042(8) 0.0304(19) Uani 1 1 d . . . . . H1D H 0.8977 0.1122 0.1604 0.036 Uiso 1 1 d R U . . . C1 C 1.0758(15) 0.1534(6) 0.0722(10) 0.036(2) Uani 1 1 d . . . . . H1A H 1.2167 0.1613 0.1605 0.054 Uiso 1 1 d R U . . . H1B H 1.0742 0.0965 0.0309 0.054 Uiso 1 1 d R U . . . H1C H 1.0595 0.1989 0.0035 0.054 Uiso 1 1 d R U . . . C2 C 0.8990(18) 0.2390(6) 0.1864(9) 0.042(2) Uani 1 1 d . . . . . H2A H 1.0372 0.2389 0.2778 0.063 Uiso 1 1 d R U . . . H2B H 0.8953 0.2900 0.1305 0.063 Uiso 1 1 d R U . . . H2C H 0.7724 0.2407 0.2047 0.063 Uiso 1 1 d R U . . . C4 C 0.475(2) 0.1354(15) -0.0347(12) 0.100(7) Uani 1 1 d . . . . . H4A H 0.3472 0.1269 -0.1301 0.149 Uiso 1 1 d R U . . . H4B H 0.4882 0.0855 0.0261 0.149 Uiso 1 1 d R U . . . H4C H 0.4528 0.1882 0.0082 0.149 Uiso 1 1 d R U . . . C3 C 0.6776(17) 0.1452(7) -0.0449(12) 0.046(3) Uani 1 1 d . . . . . H3A H 0.6978 0.0927 -0.0893 0.055 Uiso 1 1 d R U . . . H3B H 0.6628 0.1945 -0.1070 0.055 Uiso 1 1 d R 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 0.0135(2) 0.0124(3) 0.0138(2) 0.0015(2) 0.00804(16) 0.0008(2) Cd2 0.0126(2) 0.0123(3) 0.0141(2) 0.0011(2) 0.00739(16) 0.0009(2) Cl1 0.0178(6) 0.0165(7) 0.0159(6) 0.0048(5) 0.0082(4) 0.0026(5) Cl2 0.0156(5) 0.0135(6) 0.0122(5) 0.0003(5) 0.0067(4) 0.0004(5) Cl3 0.0174(5) 0.0131(6) 0.0215(6) -0.0027(5) 0.0112(4) -0.0010(5) N1 0.029(3) 0.014(3) 0.033(3) 0.005(3) 0.004(3) -0.004(2) C1 0.048(4) 0.026(4) 0.044(4) 0.005(3) 0.029(3) 0.003(3) C2 0.082(5) 0.022(4) 0.041(3) 0.003(3) 0.045(3) 0.011(4) C4 0.065(7) 0.200(19) 0.018(5) 0.001(8) 0.008(5) -0.041(10) C3 0.037(5) 0.038(5) 0.043(5) -0.001(4) 0.002(4) -0.005(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 Cl1 2.5907(15) . ? Cd1 Cl1 2.5907(15) 3_776 ? Cd1 Cl3 2.6444(16) . ? Cd1 Cl3 2.6444(16) 3_776 ? Cd1 Cl2 2.6668(17) 3_776 ? Cd1 Cl2 2.6668(17) . ? Cd1 Cd2 3.36940(16) . ? Cd1 Cd2 3.36940(14) 1_655 ? Cd2 Cl3 2.5852(17) . ? Cd2 Cl3 2.5852(17) 3_676 ? Cd2 Cl1 2.6614(18) 3_676 ? Cd2 Cl1 2.6614(18) . ? Cd2 Cl2 2.6789(14) . ? Cd2 Cl2 2.6789(14) 3_676 ? Cd2 Cd1 3.36940(15) 1_455 ? N1 C1 1.461(13) . ? N1 C2 1.462(11) . ? N1 C3 1.532(11) . ? N1 H1D 0.9001 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9599 . ? C2 H2A 0.9600 . ? C2 H2B 0.9601 . ? C2 H2C 0.9599 . ? C4 C3 1.43(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9599 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? 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 Cl1 Cd1 Cl1 180.0 . 3_776 ? Cl1 Cd1 Cl3 84.73(5) . . ? Cl1 Cd1 Cl3 95.27(5) 3_776 . ? Cl1 Cd1 Cl3 95.27(5) . 3_776 ? Cl1 Cd1 Cl3 84.73(5) 3_776 3_776 ? Cl3 Cd1 Cl3 180.00(5) . 3_776 ? Cl1 Cd1 Cl2 95.60(5) . 3_776 ? Cl1 Cd1 Cl2 84.40(5) 3_776 3_776 ? Cl3 Cd1 Cl2 97.97(5) . 3_776 ? Cl3 Cd1 Cl2 82.03(5) 3_776 3_776 ? Cl1 Cd1 Cl2 84.40(5) . . ? Cl1 Cd1 Cl2 95.60(5) 3_776 . ? Cl3 Cd1 Cl2 82.03(5) . . ? Cl3 Cd1 Cl2 97.97(5) 3_776 . ? Cl2 Cd1 Cl2 180.000(16) 3_776 . ? Cl1 Cd1 Cd2 51.02(4) . . ? Cl1 Cd1 Cd2 128.98(4) 3_776 . ? Cl3 Cd1 Cd2 49.12(4) . . ? Cl3 Cd1 Cd2 130.88(4) 3_776 . ? Cl2 Cd1 Cd2 128.91(3) 3_776 . ? Cl2 Cd1 Cd2 51.09(3) . . ? Cl1 Cd1 Cd2 128.98(4) . 1_655 ? Cl1 Cd1 Cd2 51.02(4) 3_776 1_655 ? Cl3 Cd1 Cd2 130.88(4) . 1_655 ? Cl3 Cd1 Cd2 49.12(4) 3_776 1_655 ? Cl2 Cd1 Cd2 51.09(3) 3_776 1_655 ? Cl2 Cd1 Cd2 128.91(3) . 1_655 ? Cd2 Cd1 Cd2 180.0 . 1_655 ? Cl3 Cd2 Cl3 180.0 . 3_676 ? Cl3 Cd2 Cl1 95.50(5) . 3_676 ? Cl3 Cd2 Cl1 84.50(5) 3_676 3_676 ? Cl3 Cd2 Cl1 84.50(5) . . ? Cl3 Cd2 Cl1 95.50(5) 3_676 . ? Cl1 Cd2 Cl1 180.0 3_676 . ? Cl3 Cd2 Cl2 82.90(5) . . ? Cl3 Cd2 Cl2 97.10(5) 3_676 . ? Cl1 Cd2 Cl2 97.19(5) 3_676 . ? Cl1 Cd2 Cl2 82.81(5) . . ? Cl3 Cd2 Cl2 97.10(5) . 3_676 ? Cl3 Cd2 Cl2 82.90(5) 3_676 3_676 ? Cl1 Cd2 Cl2 82.81(5) 3_676 3_676 ? Cl1 Cd2 Cl2 97.19(5) . 3_676 ? Cl2 Cd2 Cl2 180.0 . 3_676 ? Cl3 Cd2 Cd1 50.66(4) . . ? Cl3 Cd2 Cd1 129.34(4) 3_676 . ? Cl1 Cd2 Cd1 130.82(3) 3_676 . ? Cl1 Cd2 Cd1 49.18(3) . . ? Cl2 Cd2 Cd1 50.77(4) . . ? Cl2 Cd2 Cd1 129.23(4) 3_676 . ? Cl3 Cd2 Cd1 129.34(4) . 1_455 ? Cl3 Cd2 Cd1 50.66(4) 3_676 1_455 ? Cl1 Cd2 Cd1 49.18(3) 3_676 1_455 ? Cl1 Cd2 Cd1 130.82(3) . 1_455 ? Cl2 Cd2 Cd1 129.23(4) . 1_455 ? Cl2 Cd2 Cd1 50.77(4) 3_676 1_455 ? Cd1 Cd2 Cd1 180.0 . 1_455 ? Cd1 Cl1 Cd2 79.80(4) . . ? Cd1 Cl2 Cd2 78.14(4) . . ? Cd2 Cl3 Cd1 80.22(5) . . ? C1 N1 C2 112.1(7) . . ? C1 N1 C3 103.9(8) . . ? C2 N1 C3 118.1(7) . . ? C1 N1 H1D 107.5 . . ? C2 N1 H1D 107.5 . . ? C3 N1 H1D 107.3 . . ? N1 C1 H1A 109.9 . . ? N1 C1 H1B 109.3 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.2 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.2 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.7 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 C4 H4A 110.3 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 108.3 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C4 C3 N1 112.8(10) . . ? C4 C3 H3A 108.2 . . ? N1 C3 H3A 109.0 . . ? C4 C3 H3B 109.7 . . ? N1 C3 H3B 108.9 . . ? H3A C3 H3B 108.0 . . ? _refine_diff_density_max 3.583 _refine_diff_density_min -1.411 _refine_diff_density_rms 0.284 _shelx_res_file ; p21.res created by SHELXL-2014/7 TITL p21 in P2(1) New: P21/c CELL 0.71073 6.7388 15.1099 10.4269 90.000 118.749 90.000 ZERR 1 0.0003 0.0007 0.0007 0.000 0.004 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H Cd Cl N UNIT 20 0 4 12 4 L.S. 100 ACTA omit -2 4 3 omit -2 3 4 omit 2 2 1 omit 2 3 0 omit -2 1 4 omit 2 1 2 omit -2 5 2 omit -2 4 1 omit 2 5 0 omit -2 2 3 omit -2 6 1 omit -2 10 5 omit -2 3 2 omit -2 5 8 omit 2 4 1 omit 2 3 2 omit -2 9 6 omit -2 2 1 omit 2 1 0 omit -2 12 3 omit -2 13 2 omit 2 11 2 omit -2 7 4 omit -2 12 1 omit 2 4 5 omit -6 4 5 omit 2 11 0 omit -2 5 4 omit -2 6 3 omit -6 3 6 omit 2 8 5 BOND $H FMAP 2 PLAN 20 WGHT 0.000000 56.771599 FVAR 0.23543 CD1 3 1.000000 1.000000 0.500000 10.50000 0.01354 0.01238 = 0.01376 0.00150 0.00804 0.00084 CD2 3 0.500000 1.000000 0.500000 10.50000 0.01260 0.01231 = 0.01408 0.00110 0.00739 0.00093 CL1 4 0.652713 1.102059 0.358288 11.00000 0.01785 0.01653 = 0.01593 0.00484 0.00818 0.00264 CL2 4 0.917478 1.025208 0.723131 11.00000 0.01560 0.01354 = 0.01222 0.00028 0.00671 0.00044 CL3 4 0.695579 0.873460 0.436042 11.00000 0.01741 0.01313 = 0.02154 -0.00267 0.01120 -0.00103 N1 5 0.887590 0.159040 0.104163 11.00000 0.02940 0.01422 = 0.03340 0.00471 0.00385 -0.00445 AFIX 3 H1D 2 0.897680 0.112220 0.160363 11.00000 -1.20000 AFIX 0 C1 1 1.075825 0.153427 0.072235 11.00000 0.04784 0.02627 = 0.04382 0.00461 0.02941 0.00289 AFIX 3 H1A 2 1.216665 0.161267 0.160505 11.00000 -1.50000 H1B 2 1.074225 0.096477 0.030925 11.00000 -1.50000 H1C 2 1.059465 0.198857 0.003465 11.00000 -1.50000 AFIX 0 C2 1 0.898974 0.238977 0.186436 11.00000 0.08227 0.02211 = 0.04063 0.00295 0.04513 0.01078 AFIX 3 H2A 2 1.037185 0.238877 0.277807 11.00000 -1.50000 H2B 2 0.895274 0.290047 0.130546 11.00000 -1.50000 H2C 2 0.772384 0.240667 0.204746 11.00000 -1.50000 AFIX 0 C4 1 0.474549 0.135373 -0.034700 11.00000 0.06519 0.20013 = 0.01802 0.00062 0.00775 -0.04124 AFIX 3 H4A 2 0.347229 0.126873 -0.130140 11.00000 -1.50000 H4B 2 0.488199 0.085503 0.026060 11.00000 -1.50000 H4C 2 0.452829 0.188213 0.008150 11.00000 -1.50000 AFIX 0 C3 1 0.677624 0.145187 -0.044945 11.00000 0.03655 0.03790 = 0.04256 -0.00051 0.00213 -0.00461 AFIX 3 H3A 2 0.697834 0.092707 -0.089275 11.00000 -1.20000 H3B 2 0.662784 0.194487 -0.107025 11.00000 -1.20000 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 REM p21 in P2(1) New: P21/c REM R1 = 0.0683 for 1925 Fo > 4sig(Fo) and 0.0852 for all 2517 data REM 85 parameters refined using 0 restraints END WGHT 0.0000 34.6828 REM Highest difference peak 3.583, deepest hole -1.411, 1-sigma level 0.284 Q1 1 0.7555 0.9996 0.5003 11.00000 0.05 3.58 Q2 1 0.8048 0.3746 0.0587 11.00000 0.05 2.47 Q3 1 0.5895 0.9752 0.2761 11.00000 0.05 2.35 Q4 1 0.8475 0.8984 0.6390 11.00000 0.05 2.32 Q5 1 0.6347 0.1703 0.0228 11.00000 0.05 2.05 Q6 1 1.1650 0.9745 0.7239 11.00000 0.05 1.74 Q7 1 0.5507 0.8756 0.5567 11.00000 0.05 1.72 Q8 1 0.4023 0.8966 0.3624 11.00000 0.05 1.37 Q9 1 0.9394 1.1290 0.4374 11.00000 0.05 1.33 Q10 1 0.5436 0.0700 -0.0478 11.00000 0.05 1.32 Q11 1 0.6632 0.9737 0.7246 11.00000 0.05 1.30 Q12 1 0.9034 0.8972 0.3560 11.00000 0.05 1.28 Q13 1 0.9724 0.3002 0.3077 11.00000 0.05 1.09 Q14 1 0.7858 0.2026 0.2032 11.00000 0.05 1.01 Q15 1 1.2915 0.1976 0.2139 11.00000 0.05 0.99 Q16 1 0.8264 0.9721 0.3403 11.00000 0.05 0.87 Q17 1 0.7198 0.9786 0.3781 11.00000 0.05 0.87 Q18 1 1.2372 0.0836 0.1387 11.00000 0.05 0.85 Q19 1 0.3715 0.1712 0.0057 11.00000 0.05 0.84 Q20 1 0.5014 0.1947 -0.1878 11.00000 0.05 0.82 ; _shelx_res_checksum 86319 _shelx_hkl_file ; 1 0 0 0.09 0.61 2 0 0 4.42 1.24 3 0 0 -0.27 1.18 4 0 0 2247.98 61.98 5 0 0 -1.33 1.91 6 0 0 316.10 14.13 7 0 0 1.23 2.34 8 0 0 180.55 11.43 1 -1 0 0.37 0.62 2 -1 0 6.04 1.41 3 -1 0 1.89 1.29 4 -1 0 9.67 2.23 5 -1 0 0.44 1.69 6 -1 0 13.71 3.62 7 -1 0 1.22 2.33 8 -1 0 -0.69 3.28 0 2 0 2385.41 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