#------------------------------------------------------------------------------ #$Date: 2019-05-21 03:56:10 +0300 (Tue, 21 May 2019) $ #$Revision: 215336 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/10/1551071.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_1551071 loop_ _publ_author_name 'Murrie, Mark' 'Hay, Moya' 'Sarkar, Arup' 'Craig, Gavin A.' 'Bhaskaran, Lakshmi' 'Nehrkorn, Joscha' 'Ozerov, Mykhaylo' 'Marriott, Katie' 'Wilson, Claire' 'Rajaraman, Gopalan' 'Hill, Stephen' _publ_section_title ; In-depth investigation of large axial magnetic anisotropy in monometallic 3d complexes using frequency domain magnetic resonance and ab initio methods: a study of trigonal bipyramidal Co(II) ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00987F _journal_year 2019 _chemical_formula_moiety 'C12 H25 Cl3 Co1 N4' _chemical_formula_sum 'C12 H25 Cl3 Co N4' _chemical_formula_weight 390.64 _space_group_crystal_system trigonal _space_group_IT_number 155 _space_group_name_Hall 'R 3 2"' _space_group_name_H-M_alt 'R 3 2' _symmetry_space_group_name_Hall 'R 3 2"' _symmetry_space_group_name_H-M 'R 3 2 :H' _atom_sites_solution_hydrogens geom _audit_creation_date 2015-10-15 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2019-01-17 deposited with the CCDC. 2019-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 10.581(3) _cell_length_b 10.581(3) _cell_length_c 12.329(3) _cell_measurement_reflns_used 1597 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.21 _cell_measurement_theta_min 2.77 _cell_volume 1195.4(6) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 5214 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.442 _diffrn_reflns_theta_min 2.770 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.575 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1131 before and 0.0922 after correction. The Ratio of minimum to maximum transmission is 0.7196. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.628 _exptl_crystal_description needle _exptl_crystal_F_000 609 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.489 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.107 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 33 _refine_ls_number_reflns 607 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0376 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.0674 _reflns_Friedel_coverage 0.728 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 575 _reflns_number_total 607 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00987f2.cif _cod_data_source_block km555se_0m _cod_database_code 1551071 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.98(4) 0.02(4) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H) groups 3. Others Fixed Sof: H2(0.16667) 4.a Ternary CH refined with riding coordinates: N2(H2) 4.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C1(H1A,H1B) ; _shelx_res_file ; km555se_0m.res created by SHELXL-2014/7 TITL km555se_0m_a.res in R32 REM Old TITL KM555se_0m in R32 #155 REM SHELXT solution in R32 REM R1 0.054, Rweak 0.061, Alpha 0.005, Orientation as input REM Flack x = 0.016 ( 0.022 ) from Parsons' quotients REM Formula found by SHELXT: C16 Cl3 Co CELL 0.71075 10.5812 10.5812 12.3289 90 90 120 ZERR 3 0.0025 0.0025 0.0032 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM +Y,+X,-Z SYMM -Y+X,-Y,-Z SYMM -X,-X+Y,-Z SFAC C H Cl Co N UNIT 36 75 9 3 12 L.S. 5 0 0 PLAN 20 TEMP -173(2) BOND $H LIST 6 MORE -1 CONF fmap 2 53 ACTA SHEL 100 0.77 TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.028300 BASF 0.02135 FVAR 0.40221 CO1 4 0.333333 0.666667 0.666667 10.16667 0.00958 0.00958 = 0.00869 0.00000 0.00000 0.00479 CL1 3 0.553085 0.666667 0.666667 10.50000 0.01300 0.02066 = 0.01195 -0.00010 -0.00005 0.01033 N2 5 0.333333 0.666667 0.273704 10.33333 0.01262 0.01262 = 0.01037 0.00000 0.00000 0.00631 AFIX 13 H2 2 0.333332 0.666667 0.192594 10.16667 -1.20000 AFIX 0 N1 5 0.333333 0.666667 0.482695 10.33333 0.01055 0.01055 = 0.01272 0.00000 0.00000 0.00528 C2 1 0.220935 0.699462 0.315336 11.00000 0.01556 0.01540 = 0.01024 -0.00164 -0.00082 0.01051 AFIX 23 H2A 2 0.125888 0.634492 0.280221 11.00000 -1.20000 H2B 2 0.249366 0.801727 0.298280 11.00000 -1.20000 AFIX 0 C1 1 0.207287 0.675698 0.439785 11.00000 0.01296 0.01938 = 0.01016 -0.00093 -0.00084 0.00951 AFIX 23 H1A 2 0.203139 0.757578 0.475095 11.00000 -1.20000 H1B 2 0.115720 0.584399 0.456817 11.00000 -1.20000 AFIX 0 HKLF 4 REM km555se_0m_a.res in R32 REM R1 = 0.0376 for 575 Fo > 4sig(Fo) and 0.0453 for all 607 data REM 33 parameters refined using 0 restraints END WGHT 0.0283 0.0000 REM Highest difference peak 0.489, deepest hole -0.416, 1-sigma level 0.107 Q1 1 0.4626 0.7111 0.6759 11.00000 0.05 0.49 Q2 1 0.5408 0.6096 0.5946 11.00000 0.05 0.45 Q3 1 0.5435 0.8022 0.7134 11.00000 0.05 0.41 Q4 1 0.2982 0.7039 0.6131 11.00000 0.05 0.40 Q5 1 0.4683 0.4948 0.6411 11.00000 0.05 0.40 Q6 1 0.0774 0.5556 0.3841 11.00000 0.05 0.39 Q7 1 0.0228 0.4894 0.2881 11.00000 0.05 0.39 Q8 1 0.5171 0.7396 0.6844 11.00000 0.05 0.37 Q9 1 0.0543 0.5032 0.3643 11.00000 0.05 0.36 Q10 1 0.1634 0.6194 0.3788 11.00000 0.05 0.36 Q11 1 0.2130 0.6667 0.6667 10.50000 0.05 0.36 Q12 1 0.2207 0.7083 0.3817 11.00000 0.05 0.35 Q13 1 0.5900 0.5933 0.6743 11.00000 0.05 0.35 Q14 1 0.1500 0.6837 0.5095 11.00000 0.05 0.35 Q15 1 0.3365 0.9029 0.3802 11.00000 0.05 0.35 Q16 1 0.2959 0.7992 0.3756 11.00000 0.05 0.33 Q17 1 -0.0593 0.5328 0.2895 11.00000 0.05 0.33 Q18 1 0.5848 0.7509 0.6024 11.00000 0.05 0.32 Q19 1 0.6105 0.7740 0.6767 11.00000 0.05 0.32 Q20 1 0.6758 0.6667 0.6667 10.50000 0.05 0.32 ; _shelx_res_checksum 14555 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 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 Co1 Co 0.3333 0.6667 0.6667 0.0093(4) Uani 1 6 d S T P Cl1 Cl 0.55309(12) 0.6667 0.6667 0.0144(4) Uani 1 2 d S T P N2 N 0.3333 0.6667 0.2737(4) 0.0119(11) Uani 1 3 d S T P H2 H 0.3333 0.6667 0.1926 0.014 Uiso 0.5 3 calc RS T P N1 N 0.3333 0.6667 0.4827(4) 0.0113(11) Uani 1 3 d S T P C2 C 0.2209(4) 0.6995(4) 0.3153(3) 0.0125(9) Uani 1 1 d . . . H2A H 0.1259 0.6345 0.2802 0.015 Uiso 1 1 calc R . . H2B H 0.2494 0.8017 0.2983 0.015 Uiso 1 1 calc R . . C1 C 0.2073(4) 0.6757(4) 0.4398(3) 0.0135(9) Uani 1 1 d . . . H1A H 0.2031 0.7576 0.4751 0.016 Uiso 1 1 calc R . . H1B H 0.1157 0.5844 0.4568 0.016 Uiso 1 1 calc 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 Co1 0.0096(5) 0.0096(5) 0.0087(6) 0.000 0.000 0.0048(2) Cl1 0.0130(6) 0.0207(8) 0.0120(7) -0.0001(5) 0.0000(3) 0.0103(4) N2 0.0126(17) 0.0126(17) 0.010(2) 0.000 0.000 0.0063(8) N1 0.0106(16) 0.0106(16) 0.013(3) 0.000 0.000 0.0053(8) C2 0.0156(19) 0.015(2) 0.0102(16) -0.0016(15) -0.0008(14) 0.0105(17) C1 0.0130(19) 0.019(2) 0.0102(19) -0.0009(15) -0.0008(15) 0.0095(15) 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' Co Co 0.3494 0.9721 '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' 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 Cl1 Co1 Cl1 120.000(1) 2_665 . Cl1 Co1 Cl1 120.0 2_665 3_565 Cl1 Co1 Cl1 120.0 3_565 . N1 Co1 Cl1 90.001(1) . 3_565 N1 Co1 Cl1 89.999(1) 10_456 3_565 N1 Co1 Cl1 90.000 10_456 . N1 Co1 Cl1 90.0 10_456 2_665 N1 Co1 Cl1 90.0 . 2_665 N1 Co1 Cl1 90.000 . . N1 Co1 N1 180.0 10_456 . C2 N2 H2 110.2 . . C2 N2 H2 110.2 3_565 . C2 N2 H2 110.2 2_665 . C2 N2 C2 108.7(2) . 3_565 C2 N2 C2 108.7(2) . 2_665 C2 N2 C2 108.7(2) 3_565 2_665 C1 N1 Co1 110.9(2) . . C1 N1 Co1 110.9(2) 2_665 . C1 N1 Co1 110.9(2) 3_565 . C1 N1 C1 108.0(2) 3_565 2_665 C1 N1 C1 108.0(2) . 3_565 C1 N1 C1 108.0(2) . 2_665 N2 C2 H2A 109.9 . . N2 C2 H2B 109.9 . . N2 C2 C1 108.9(3) . . H2A C2 H2B 108.3 . . C1 C2 H2A 109.9 . . C1 C2 H2B 109.9 . . N1 C1 C2 110.5(3) . . N1 C1 H1A 109.6 . . N1 C1 H1B 109.6 . . C2 C1 H1A 109.6 . . C2 C1 H1B 109.6 . . H1A C1 H1B 108.1 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co1 Cl1 2.3252(14) . Co1 Cl1 2.3253(14) 2_665 Co1 Cl1 2.3253(14) 3_565 Co1 N1 2.268(5) 10_456 Co1 N1 2.268(5) . N2 H2 1.0000 . N2 C2 1.487(4) . N2 C2 1.487(4) 3_565 N2 C2 1.487(4) 2_665 N1 C1 1.482(4) 3_565 N1 C1 1.482(4) 2_665 N1 C1 1.482(4) . C2 H2A 0.9900 . C2 H2B 0.9900 . C2 C1 1.550(5) . C1 H1A 0.9900 . C1 H1B 0.9900 . 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 Co1 N1 C1 C2 171.3(2) . N2 C2 C1 N1 14.9(4) . C2 N2 C2 C1 50.6(4) 2_665 C2 N2 C2 C1 -67.6(3) 3_565 C1 N1 C1 C2 -66.9(3) 2_665 C1 N1 C1 C2 49.6(4) 3_565 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.98(4) 2 0.02(4)