#------------------------------------------------------------------------------ #$Date: 2023-12-12 01:40:41 +0200 (Tue, 12 Dec 2023) $ #$Revision: 288230 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247849.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247849 loop_ _publ_author_name 'Li, Hai Tao' 'Guo, Zhenwei' 'Liu, Tie' 'Xin, Lianxin' 'Guo, Fang' _publ_section_title ; Solid-State Reaction among [CoCl4]2-, [CuCl4]2- and [CuCl4(H2O)]2-ions through Transmetalation and Liquid-Assisted Grinding ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01038D _journal_year 2024 _chemical_formula_moiety '2(Cl4 Cu H2 O), C14 H22 N4' _chemical_formula_sum 'C14 H26 Cl8 Cu2 N4 O2' _chemical_formula_weight 693.07 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2023-10-30 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-10-30 deposited with the CCDC. 2023-12-06 downloaded from the CCDC. ; _cell_angle_alpha 74.548(2) _cell_angle_beta 88.019(2) _cell_angle_gamma 80.640(2) _cell_formula_units_Z 1 _cell_length_a 6.3666(3) _cell_length_b 9.1403(5) _cell_length_c 11.6139(6) _cell_measurement_reflns_used 9308 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 30.60 _cell_measurement_theta_min 2.56 _cell_volume 642.71(6) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_unetI/netI 0.0186 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9903 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.019 _diffrn_reflns_theta_min 2.342 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.506 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.4763 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1074 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.6384. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.791 _exptl_crystal_description plate _exptl_crystal_F_000 348 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.838 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 2270 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0256 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.8163P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0651 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2157 _reflns_number_total 2270 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01038d2.cif _cod_data_source_block 231030_l1_0m_a _cod_database_code 7247849 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.634 _shelx_estimated_absorpt_t_min 0.573 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances H1B-H2A 2.8 with sigma of 0.01 3.a Rotating group: O1(H1B,H1C) 3.b Secondary CH2 refined with riding coordinates: N2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B) 3.c Aromatic/amide H refined with riding coordinates: N1(H1), C1(H1A), C2(H2), C4(H4), C5(H5) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Cu1 Cu 0.44124(5) 0.75343(4) 0.70166(3) 0.02792(11) Uani 1 1 d . . . . . Cl1 Cl 0.50287(12) 0.87093(9) 0.84632(6) 0.04351(19) Uani 1 1 d . . . . . Cl2 Cl 0.29700(10) 0.85604(7) 0.50223(6) 0.03278(16) Uani 1 1 d . . . . . Cl3 Cl 0.58073(9) 0.48810(7) 0.69948(6) 0.03059(15) Uani 1 1 d . . . . . Cl4 Cl 0.12795(10) 0.69363(9) 0.78442(6) 0.03997(18) Uani 1 1 d . . . . . O1 O 0.7187(3) 0.8016(2) 0.62425(15) 0.0264(4) Uani 1 1 d . . . . . H1B H 0.831100 0.768869 0.675998 0.040 Uiso 1 1 d DR U . . . H1C H 0.722229 0.904426 0.600315 0.040 Uiso 1 1 d R U . . . N1 N 1.1193(4) 0.7885(3) 0.03043(19) 0.0338(5) Uani 1 1 d . . . . . H1 H 1.183874 0.787644 -0.035730 0.041 Uiso 1 1 calc R U . . . N2 N 0.7547(3) 0.6365(2) 0.42680(18) 0.0270(4) Uani 1 1 d . . . . . H2A H 0.698790 0.646923 0.496018 0.032 Uiso 1 1 calc DR U . . . H2B H 0.651818 0.618258 0.385084 0.032 Uiso 1 1 calc R U . . . C1 C 1.1901(4) 0.8632(3) 0.1015(2) 0.0337(6) Uani 1 1 d . . . . . H1A H 1.305851 0.914486 0.078775 0.040 Uiso 1 1 calc R U . . . C2 C 1.0916(4) 0.8642(3) 0.2082(2) 0.0307(6) Uani 1 1 d . . . . . H2 H 1.139377 0.916953 0.257773 0.037 Uiso 1 1 calc R U . . . C3 C 0.9201(4) 0.7862(3) 0.2419(2) 0.0251(5) Uani 1 1 d . . . . . C4 C 0.8490(5) 0.7130(3) 0.1641(2) 0.0343(6) Uani 1 1 d . . . . . H4 H 0.731656 0.662676 0.183613 0.041 Uiso 1 1 calc R U . . . C5 C 0.9522(5) 0.7149(3) 0.0580(2) 0.0386(7) Uani 1 1 d . . . . . H5 H 0.905930 0.665164 0.005665 0.046 Uiso 1 1 calc R U . . . C6 C 0.8166(4) 0.7874(3) 0.3605(2) 0.0312(6) Uani 1 1 d . . . . . H6A H 0.914247 0.815991 0.409873 0.037 Uiso 1 1 calc R U . . . H6B H 0.690474 0.865412 0.347050 0.037 Uiso 1 1 calc R U . . . C7 C 0.9228(4) 0.4971(3) 0.4532(2) 0.0289(5) Uani 1 1 d . . . . . H7A H 0.999285 0.490580 0.380590 0.035 Uiso 1 1 calc R U . . . H7B H 0.856483 0.405783 0.481126 0.035 Uiso 1 1 calc 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 Cu1 0.02259(17) 0.0413(2) 0.02611(18) -0.01750(14) 0.00671(12) -0.00998(13) Cl1 0.0443(4) 0.0667(5) 0.0364(4) -0.0322(4) 0.0148(3) -0.0293(4) Cl2 0.0381(4) 0.0319(3) 0.0276(3) -0.0010(3) -0.0082(3) -0.0132(3) Cl3 0.0255(3) 0.0258(3) 0.0392(4) -0.0064(3) 0.0059(3) -0.0053(2) Cl4 0.0248(3) 0.0722(5) 0.0336(4) -0.0278(3) 0.0100(3) -0.0175(3) O1 0.0255(9) 0.0299(9) 0.0252(9) -0.0080(7) 0.0034(7) -0.0083(7) N1 0.0406(13) 0.0383(12) 0.0225(11) -0.0080(10) 0.0129(10) -0.0094(10) N2 0.0257(10) 0.0354(12) 0.0188(10) -0.0061(9) 0.0050(8) -0.0045(9) C1 0.0331(14) 0.0376(15) 0.0311(14) -0.0063(12) 0.0075(11) -0.0142(12) C2 0.0343(14) 0.0336(14) 0.0276(13) -0.0107(11) 0.0032(11) -0.0115(11) C3 0.0285(12) 0.0252(12) 0.0206(12) -0.0055(10) 0.0043(10) -0.0029(10) C4 0.0385(15) 0.0422(15) 0.0280(14) -0.0123(12) 0.0093(11) -0.0196(12) C5 0.0512(17) 0.0454(16) 0.0269(14) -0.0169(12) 0.0074(12) -0.0194(14) C6 0.0385(14) 0.0317(14) 0.0258(13) -0.0110(11) 0.0101(11) -0.0088(11) C7 0.0307(13) 0.0319(13) 0.0255(13) -0.0088(11) 0.0016(11) -0.0070(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Cu1 Cl2 131.62(3) . . ? Cl1 Cu1 Cl3 126.42(3) . . ? Cl2 Cu1 Cl3 100.89(2) . . ? Cl4 Cu1 Cl1 92.32(3) . . ? Cl4 Cu1 Cl2 94.45(3) . . ? Cl4 Cu1 Cl3 93.60(3) . . ? O1 Cu1 Cl1 89.72(5) . . ? O1 Cu1 Cl2 84.47(5) . . ? O1 Cu1 Cl3 84.89(5) . . ? O1 Cu1 Cl4 177.93(5) . . ? Cu1 O1 H1B 112.9 . . ? Cu1 O1 H1C 112.4 . . ? H1B O1 H1C 101.0 . . ? C1 N1 H1 118.7 . . ? C1 N1 C5 122.6(2) . . ? C5 N1 H1 118.7 . . ? H2A N2 H2B 107.1 . . ? C6 N2 H2A 107.7 . . ? C6 N2 H2B 107.7 . . ? C7 N2 H2A 107.7 . . ? C7 N2 H2B 107.7 . . ? C7 N2 C6 118.4(2) . . ? N1 C1 H1A 120.1 . . ? N1 C1 C2 119.7(2) . . ? C2 C1 H1A 120.1 . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.8(2) . . ? C3 C2 H2 120.1 . . ? C2 C3 C6 118.7(2) . . ? C4 C3 C2 118.5(2) . . ? C4 C3 C6 122.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.8(2) . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 119.6(3) . . ? N1 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N2 C6 C3 113.8(2) . . ? N2 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C3 C6 H6A 108.8 . . ? C3 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C7 111.0(3) . 2_766 ? N2 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C7 C7 H7A 109.4 2_766 . ? C7 C7 H7B 109.4 2_766 . ? H7A C7 H7B 108.0 . . ? 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 Cu1 Cl1 2.2966(7) . ? Cu1 Cl2 2.4076(7) . ? Cu1 Cl3 2.4497(7) . ? Cu1 Cl4 2.2678(7) . ? Cu1 O1 2.0137(16) . ? O1 H1B 0.9094 . ? O1 H1C 0.9102 . ? N1 H1 0.8600 . ? N1 C1 1.333(4) . ? N1 C5 1.335(4) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 C6 1.497(3) . ? N2 C7 1.495(3) . ? C1 H1A 0.9300 . ? C1 C2 1.371(4) . ? C2 H2 0.9300 . ? C2 C3 1.389(4) . ? C3 C4 1.386(4) . ? C3 C6 1.507(3) . ? C4 H4 0.9300 . ? C4 C5 1.374(4) . ? C5 H5 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C7 1.507(5) 2_766 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.6(4) . . . . ? C1 N1 C5 C4 -1.0(4) . . . . ? C1 C2 C3 C4 -2.0(4) . . . . ? C1 C2 C3 C6 179.2(2) . . . . ? C2 C3 C4 C5 2.0(4) . . . . ? C2 C3 C6 N2 -140.0(2) . . . . ? C3 C4 C5 N1 -0.5(5) . . . . ? C4 C3 C6 N2 41.2(4) . . . . ? C5 N1 C1 C2 0.9(4) . . . . ? C6 N2 C7 C7 70.8(3) . . . 2_766 ? C6 C3 C4 C5 -179.3(3) . . . . ? C7 N2 C6 C3 56.0(3) . . . . ?