#------------------------------------------------------------------------------ #$Date: 2020-04-24 01:50:12 +0300 (Fri, 24 Apr 2020) $ #$Revision: 251115 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240386.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_7240386 loop_ _publ_author_name 'Yang, Chih-Tung' 'Yang, Xiang-Kai' 'Hu, Ji-Hong' 'Lee, Wei-Te' 'Chen, Tsun-Ren' 'Wang, Chih-Chieh' 'Chen, Jhy-Der' _publ_section_title ; One-dimensional chains based on linear tetranuclear copper(I) units: reversible structural transformation and luminescence change ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00294A _journal_year 2020 _chemical_formula_sum 'C25 H25 Br2 Cu4 N9 O' _chemical_formula_weight 881.52 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-04-09 deposited with the CCDC. 2020-04-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.5350(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.08960(10) _cell_length_b 13.6597(2) _cell_length_c 17.8304(2) _cell_measurement_reflns_used 9877 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.61 _cell_measurement_theta_min 2.28 _cell_volume 2885.05(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _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 0.0342 _diffrn_reflns_av_unetI/netI 0.0526 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 26474 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.292 _diffrn_reflns_theta_min 1.719 _exptl_absorpt_coefficient_mu 5.717 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.029 _exptl_crystal_description block _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.031 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 7107 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0422 _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^)+(0.0440P)^2^+1.8004P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.1064 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4253 _reflns_number_total 7107 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00294a2.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'multi_scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7240386 _shelx_shelxl_version_number 2014/7 _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_min 0.279 _shelx_estimated_absorpt_t_max 0.763 _shelx_res_file ; 12013_0m.res created by SHELXL-2014/7 TITL 12013_0m in P2(1)/c CELL 0.71073 12.0896 13.6597 17.8304 90.000 101.535 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CU BR O UNIT 100 100 36 16 8 4 TEMP 23.000 SIZE 0.05 0.20 0.30 acta L.S. 4 BOND $H FMAP 2 PLAN 20 WGHT 0.044000 1.800400 FVAR 0.05459 CU1 4 0.736351 0.518156 0.699166 11.00000 0.04643 0.05990 = 0.03162 0.00041 0.00531 -0.00749 CU2 4 0.571809 0.436911 0.735517 11.00000 0.04168 0.07828 = 0.02331 -0.00110 0.00336 -0.01011 CU3 4 0.404392 0.360375 0.771863 11.00000 0.04264 0.07976 = 0.02338 0.00275 0.00285 -0.01262 CU4 4 0.248593 0.264248 0.807141 11.00000 0.04728 0.06249 = 0.03207 0.00452 0.00595 -0.00822 BR1 5 0.881001 0.630699 0.655675 11.00000 0.04492 0.04791 = 0.04300 -0.00179 0.01548 -0.00129 BR2 5 0.408975 0.144108 0.771258 11.00000 0.04750 0.03812 = 0.03710 0.00050 0.01105 0.00033 N1 3 0.669924 0.443438 0.599718 11.00000 0.04236 0.03510 = 0.02785 0.00006 0.00773 0.00164 N2 3 0.498714 0.408660 0.632496 11.00000 0.03981 0.03642 = 0.02546 -0.00154 0.00323 -0.00430 N3 3 0.329896 0.371449 0.667553 11.00000 0.04194 0.04104 = 0.02689 0.00344 0.00220 -0.00495 N4 3 0.168088 0.307617 0.700342 11.00000 0.04056 0.04095 = 0.03357 0.00767 0.00690 0.00290 N5 3 0.813657 0.462423 0.804100 11.00000 0.03912 0.05854 = 0.03741 0.01491 0.00499 0.00306 N6 3 0.647637 0.411744 0.838410 11.00000 0.04095 0.03995 = 0.02442 -0.00260 0.00293 -0.00406 N7 3 0.480621 0.374258 0.875498 11.00000 0.04455 0.03962 = 0.02206 0.00009 0.00686 -0.00446 N8 3 0.315193 0.324419 0.910700 11.00000 0.04701 0.03704 = 0.02910 0.00161 0.01311 -0.00030 C1 1 0.741974 0.437073 0.551053 11.00000 0.04941 0.04081 = 0.03627 0.00007 0.00850 0.00259 AFIX 43 H1A 2 0.814487 0.461998 0.566814 11.00000 -1.20000 AFIX 0 C2 1 0.714036 0.395772 0.479484 11.00000 0.05872 0.05701 = 0.03749 -0.00366 0.01734 0.00652 AFIX 43 H2A 2 0.767082 0.390136 0.448468 11.00000 -1.20000 AFIX 0 C3 1 0.604571 0.362843 0.455011 11.00000 0.06842 0.04734 = 0.02828 -0.00887 0.00664 -0.00393 AFIX 43 H3A 2 0.582080 0.336837 0.406133 11.00000 -1.20000 AFIX 0 C4 1 0.529913 0.368639 0.502714 11.00000 0.05278 0.04020 = 0.03221 -0.00426 0.00618 -0.00504 AFIX 43 H4A 2 0.456088 0.346964 0.486432 11.00000 -1.20000 AFIX 0 C5 1 0.564724 0.407510 0.576723 11.00000 0.04315 0.02791 = 0.02302 0.00535 0.00341 0.00166 C6 1 0.391397 0.385134 0.614334 11.00000 0.04483 0.03290 = 0.02332 0.00562 0.00047 0.00040 AFIX 43 H6A 2 0.357532 0.377856 0.563018 11.00000 -1.20000 AFIX 0 C7 1 0.215451 0.349941 0.646643 11.00000 0.04047 0.03609 = 0.03133 -0.00100 0.00087 0.00481 C8 1 0.150252 0.371436 0.573809 11.00000 0.04768 0.05365 = 0.03675 0.01228 0.00061 0.00181 AFIX 43 H8A 2 0.182629 0.404221 0.537863 11.00000 -1.20000 AFIX 0 C9 1 0.039835 0.344165 0.556121 11.00000 0.04480 0.08687 = 0.04856 0.01588 -0.00561 0.00672 AFIX 43 H9A 2 -0.002619 0.355924 0.507425 11.00000 -1.20000 AFIX 0 C10 1 -0.008443 0.299441 0.610161 11.00000 0.03404 0.09292 = 0.06486 0.01973 -0.00636 -0.00271 AFIX 43 H10A 2 -0.083801 0.280366 0.599187 11.00000 -1.20000 AFIX 0 C11 1 0.058193 0.283430 0.681640 11.00000 0.03818 0.07093 = 0.05751 0.02016 0.00632 -0.00154 AFIX 43 H11A 2 0.025172 0.254296 0.718890 11.00000 -1.20000 AFIX 0 C12 1 0.926712 0.472401 0.819085 11.00000 0.04161 0.12285 = 0.07104 0.04843 0.00779 -0.00018 AFIX 43 H12A 2 0.960589 0.501093 0.782076 11.00000 -1.20000 AFIX 0 C13 1 0.994843 0.442115 0.886722 11.00000 0.04181 0.16657 = 0.10357 0.08726 -0.00142 -0.00339 AFIX 43 H13A 2 1.072618 0.451179 0.895653 11.00000 -1.20000 AFIX 0 C14 1 0.944835 0.398794 0.939649 11.00000 0.04678 0.14420 = 0.07774 0.05875 -0.01017 0.00494 AFIX 43 H14A 2 0.988693 0.376882 0.985467 11.00000 -1.20000 AFIX 0 C15 1 0.831211 0.387192 0.926215 11.00000 0.05364 0.07979 = 0.04671 0.02590 0.00275 0.00234 AFIX 43 H15A 2 0.797342 0.356968 0.962587 11.00000 -1.20000 AFIX 0 C16 1 0.764928 0.420752 0.857541 11.00000 0.04086 0.04385 = 0.03359 0.00213 0.00131 0.00427 C17 1 0.590826 0.390630 0.892261 11.00000 0.04825 0.03250 = 0.02431 -0.00309 0.00131 -0.00173 AFIX 43 H17A 2 0.628874 0.387174 0.942967 11.00000 -1.20000 AFIX 0 C18 1 0.419925 0.360809 0.933079 11.00000 0.05101 0.02324 = 0.02921 0.00276 0.00921 -0.00060 C19 1 0.462267 0.385191 1.010506 11.00000 0.06654 0.04078 = 0.02678 -0.00046 0.00817 -0.00703 AFIX 43 H19A 2 0.536049 0.407489 1.025619 11.00000 -1.20000 AFIX 0 C20 1 0.394760 0.376024 1.063340 11.00000 0.09612 0.04252 = 0.02637 -0.00442 0.01882 -0.00721 AFIX 43 H20A 2 0.422125 0.391799 1.114421 11.00000 -1.20000 AFIX 0 C21 1 0.286254 0.343233 1.039701 11.00000 0.08661 0.04186 = 0.04553 -0.00284 0.03738 -0.00499 AFIX 43 H21A 2 0.237843 0.338810 1.074060 11.00000 -1.20000 AFIX 0 C22 1 0.249919 0.316804 0.963821 11.00000 0.05710 0.04289 = 0.04409 0.00010 0.02050 -0.00079 AFIX 43 H22A 2 0.176976 0.292601 0.948603 11.00000 -1.20000 AFIX 0 O 6 -0.260865 0.107749 0.584822 11.00000 0.11445 0.48884 = 0.05823 0.01494 0.01654 -0.03424 N9 3 -0.246583 0.134836 0.706829 11.00000 0.07748 0.04650 = 0.05308 0.01116 0.01901 0.01466 C23 1 -0.232770 0.066735 0.657062 11.00000 0.13626 0.09671 = 0.45576 -0.09584 0.15482 -0.01146 AFIX 43 H23A 2 -0.208569 0.002839 0.668457 11.00000 -1.20000 AFIX 0 C24 1 -0.230943 0.121432 0.785652 11.00000 0.16613 0.46393 = 0.06453 0.04006 0.00992 -0.08479 AFIX 137 H24A 2 -0.193768 0.060004 0.799316 11.00000 -1.50000 H24B 2 -0.302921 0.121397 0.800637 11.00000 -1.50000 H24C 2 -0.185353 0.173652 0.811356 11.00000 -1.50000 AFIX 0 C25 1 -0.288465 0.218483 0.681740 11.00000 0.23147 AFIX 137 H25A 2 -0.290470 0.222998 0.627755 11.00000 -1.50000 H25B 2 -0.242336 0.270179 0.707774 11.00000 -1.50000 H25C 2 -0.363687 0.224385 0.691062 11.00000 -1.50000 AFIX 0 HKLF 4 REM 12013_0m in P2(1)/c REM R1 = 0.0422 for 4253 Fo > 4sig(Fo) and 0.0926 for all 7107 data REM 367 parameters refined using 0 restraints END WGHT 0.0440 1.8005 REM Highest difference peak 1.031, deepest hole -0.731, 1-sigma level 0.100 Q1 1 -0.2669 0.1578 0.6371 11.00000 0.05 1.03 Q2 1 -0.2476 0.0747 0.5874 11.00000 0.05 0.90 Q3 1 -0.2204 0.0435 0.7436 11.00000 0.05 0.72 Q4 1 -0.2254 0.2230 0.7641 11.00000 0.05 0.72 Q5 1 -0.4337 0.2743 0.7369 11.00000 0.05 0.64 Q6 1 -0.4137 0.0749 0.7324 11.00000 0.05 0.58 Q7 1 -0.1330 0.0836 0.6521 11.00000 0.05 0.57 Q8 1 0.4809 0.3602 0.7950 11.00000 0.05 0.54 Q9 1 -0.2579 -0.0271 0.6986 11.00000 0.05 0.51 Q10 1 -0.2918 0.2031 0.5864 11.00000 0.05 0.43 Q11 1 0.8141 0.6299 0.6385 11.00000 0.05 0.42 Q12 1 0.4239 0.1374 0.8066 11.00000 0.05 0.39 Q13 1 0.4795 0.1240 0.7718 11.00000 0.05 0.39 Q14 1 0.3366 0.3480 0.7717 11.00000 0.05 0.38 Q15 1 0.4280 0.3008 0.7707 11.00000 0.05 0.37 Q16 1 0.3464 0.1441 0.7503 11.00000 0.05 0.35 Q17 1 0.6543 0.4281 0.7562 11.00000 0.05 0.35 Q18 1 0.2063 0.1839 0.7932 11.00000 0.05 0.34 Q19 1 0.2679 0.3627 0.6511 11.00000 0.05 0.34 Q20 1 0.3584 0.4009 0.7006 11.00000 0.05 0.33 ; _shelx_res_checksum 98885 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' 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 0.73635(4) 0.51816(5) 0.69917(3) 0.04633(17) Uani 1 1 d . . . . . Cu2 Cu 0.57181(4) 0.43691(5) 0.73552(3) 0.04819(17) Uani 1 1 d . . . . . Cu3 Cu 0.40439(4) 0.36038(5) 0.77186(3) 0.04912(18) Uani 1 1 d . . . . . Cu4 Cu 0.24859(4) 0.26425(5) 0.80714(3) 0.04755(17) Uani 1 1 d . . . . . Br1 Br 0.88100(4) 0.63070(3) 0.65567(2) 0.04435(14) Uani 1 1 d . . . . . Br2 Br 0.40898(4) 0.14411(3) 0.77126(2) 0.04054(13) Uani 1 1 d . . . . . N1 N 0.6699(3) 0.4434(2) 0.59972(16) 0.0350(8) Uani 1 1 d . . . . . N2 N 0.4987(3) 0.4087(3) 0.63250(16) 0.0344(8) Uani 1 1 d . . . . . N3 N 0.3299(3) 0.3714(2) 0.66755(17) 0.0373(9) Uani 1 1 d . . . . . N4 N 0.1681(3) 0.3076(3) 0.70034(17) 0.0384(8) Uani 1 1 d . . . . . N5 N 0.8137(3) 0.4624(3) 0.80410(18) 0.0454(9) Uani 1 1 d . . . . . N6 N 0.6476(3) 0.4117(3) 0.83841(16) 0.0356(8) Uani 1 1 d . . . . . N7 N 0.4806(3) 0.3743(2) 0.87550(16) 0.0354(8) Uani 1 1 d . . . . . N8 N 0.3152(3) 0.3244(3) 0.91070(17) 0.0370(8) Uani 1 1 d . . . . . C1 C 0.7420(4) 0.4371(3) 0.5511(2) 0.0422(11) Uani 1 1 d . . . . . H1A H 0.8145 0.4620 0.5668 0.051 Uiso 1 1 calc R U . . . C2 C 0.7140(4) 0.3958(4) 0.4795(2) 0.0500(12) Uani 1 1 d . . . . . H2A H 0.7671 0.3901 0.4485 0.060 Uiso 1 1 calc R U . . . C3 C 0.6046(4) 0.3628(3) 0.4550(2) 0.0484(12) Uani 1 1 d . . . . . H3A H 0.5821 0.3368 0.4061 0.058 Uiso 1 1 calc R U . . . C4 C 0.5299(4) 0.3686(3) 0.5027(2) 0.0421(11) Uani 1 1 d . . . . . H4A H 0.4561 0.3470 0.4864 0.050 Uiso 1 1 calc R U . . . C5 C 0.5647(3) 0.4075(3) 0.57672(19) 0.0318(9) Uani 1 1 d . . . . . C6 C 0.3914(3) 0.3851(3) 0.6143(2) 0.0346(10) Uani 1 1 d . . . . . H6A H 0.3575 0.3779 0.5630 0.041 Uiso 1 1 calc R U . . . C7 C 0.2155(3) 0.3499(3) 0.6466(2) 0.0368(10) Uani 1 1 d . . . . . C8 C 0.1503(4) 0.3714(3) 0.5738(2) 0.0471(12) Uani 1 1 d . . . . . H8A H 0.1826 0.4042 0.5379 0.057 Uiso 1 1 calc R U . . . C9 C 0.0398(4) 0.3442(4) 0.5561(3) 0.0622(15) Uani 1 1 d . . . . . H9A H -0.0026 0.3559 0.5074 0.075 Uiso 1 1 calc R U . . . C10 C -0.0084(4) 0.2994(4) 0.6102(3) 0.0662(16) Uani 1 1 d . . . . . H10A H -0.0838 0.2804 0.5992 0.079 Uiso 1 1 calc R U . . . C11 C 0.0582(4) 0.2834(4) 0.6816(3) 0.0560(13) Uani 1 1 d . . . . . H11A H 0.0252 0.2543 0.7189 0.067 Uiso 1 1 calc R U . . . C12 C 0.9267(4) 0.4724(5) 0.8191(3) 0.0790(19) Uani 1 1 d . . . . . H12A H 0.9606 0.5011 0.7821 0.095 Uiso 1 1 calc R U . . . C13 C 0.9948(5) 0.4421(6) 0.8867(4) 0.106(3) Uani 1 1 d . . . . . H13A H 1.0726 0.4512 0.8957 0.127 Uiso 1 1 calc R U . . . C14 C 0.9448(5) 0.3988(5) 0.9396(3) 0.093(2) Uani 1 1 d . . . . . H14A H 0.9887 0.3769 0.9855 0.111 Uiso 1 1 calc R U . . . C15 C 0.8312(4) 0.3872(4) 0.9262(3) 0.0611(14) Uani 1 1 d . . . . . H15A H 0.7973 0.3570 0.9626 0.073 Uiso 1 1 calc R U . . . C16 C 0.7649(3) 0.4208(3) 0.8575(2) 0.0403(10) Uani 1 1 d . . . . . C17 C 0.5908(4) 0.3906(3) 0.8923(2) 0.0358(10) Uani 1 1 d . . . . . H17A H 0.6289 0.3872 0.9430 0.043 Uiso 1 1 calc R U . . . C18 C 0.4199(4) 0.3608(3) 0.9331(2) 0.0343(10) Uani 1 1 d . . . . . C19 C 0.4623(4) 0.3852(3) 1.0105(2) 0.0449(12) Uani 1 1 d . . . . . H19A H 0.5360 0.4075 1.0256 0.054 Uiso 1 1 calc R U . . . C20 C 0.3948(5) 0.3760(3) 1.0633(2) 0.0541(14) Uani 1 1 d . . . . . H20A H 0.4221 0.3918 1.1144 0.065 Uiso 1 1 calc R U . . . C21 C 0.2863(5) 0.3432(3) 1.0397(3) 0.0546(13) Uani 1 1 d . . . . . H21A H 0.2378 0.3388 1.0741 0.066 Uiso 1 1 calc R U . . . C22 C 0.2499(4) 0.3168(3) 0.9638(2) 0.0466(11) Uani 1 1 d . . . . . H22A H 0.1770 0.2926 0.9486 0.056 Uiso 1 1 calc R U . . . O O -0.2609(6) 0.1077(8) 0.5848(3) 0.221(5) Uani 1 1 d . . . . . N9 N -0.2466(4) 0.1348(3) 0.7068(2) 0.0582(11) Uani 1 1 d . . . . . C23 C -0.2328(8) 0.0667(7) 0.6571(10) 0.216(7) Uani 1 1 d . . . . . H23A H -0.2086 0.0028 0.6685 0.260 Uiso 1 1 calc R U . . . C24 C -0.2309(8) 0.1214(10) 0.7857(4) 0.233(8) Uani 1 1 d . . . . . H24A H -0.1938 0.0600 0.7993 0.350 Uiso 1 1 calc R U . . . H24B H -0.3029 0.1214 0.8006 0.350 Uiso 1 1 calc R U . . . H24C H -0.1854 0.1737 0.8114 0.350 Uiso 1 1 calc R U . . . C25 C -0.2885(10) 0.2185(11) 0.6817(6) 0.231(6) Uiso 1 1 d . . . . . H25A H -0.2905 0.2230 0.6278 0.347 Uiso 1 1 calc R U . . . H25B H -0.2423 0.2702 0.7078 0.347 Uiso 1 1 calc R U . . . H25C H -0.3637 0.2244 0.6911 0.347 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 0.0464(3) 0.0599(4) 0.0316(3) 0.0004(3) 0.0053(2) -0.0075(3) Cu2 0.0417(3) 0.0783(5) 0.0233(2) -0.0011(3) 0.0034(2) -0.0101(3) Cu3 0.0426(3) 0.0798(5) 0.0234(3) 0.0028(3) 0.0028(2) -0.0126(3) Cu4 0.0473(3) 0.0625(4) 0.0321(3) 0.0045(3) 0.0059(2) -0.0082(3) Br1 0.0449(3) 0.0479(3) 0.0430(2) -0.0018(2) 0.0155(2) -0.0013(2) Br2 0.0475(3) 0.0381(3) 0.0371(2) 0.00050(19) 0.01105(19) 0.0003(2) N1 0.042(2) 0.035(2) 0.0278(16) 0.0001(15) 0.0077(15) 0.0016(17) N2 0.040(2) 0.036(2) 0.0255(16) -0.0015(15) 0.0032(14) -0.0043(16) N3 0.042(2) 0.041(2) 0.0269(17) 0.0034(15) 0.0022(15) -0.0049(17) N4 0.041(2) 0.041(2) 0.0336(18) 0.0077(16) 0.0069(15) 0.0029(17) N5 0.039(2) 0.059(3) 0.0374(19) 0.0149(18) 0.0050(16) 0.0031(18) N6 0.041(2) 0.040(2) 0.0244(16) -0.0026(15) 0.0029(14) -0.0041(17) N7 0.045(2) 0.040(2) 0.0221(16) 0.0001(14) 0.0069(14) -0.0045(16) N8 0.047(2) 0.037(2) 0.0291(17) 0.0016(15) 0.0131(15) -0.0003(17) C1 0.049(3) 0.041(3) 0.036(2) 0.000(2) 0.0085(19) 0.003(2) C2 0.059(3) 0.057(3) 0.037(2) -0.004(2) 0.017(2) 0.007(3) C3 0.068(3) 0.047(3) 0.028(2) -0.009(2) 0.007(2) -0.004(2) C4 0.053(3) 0.040(3) 0.032(2) -0.0043(19) 0.0062(19) -0.005(2) C5 0.043(2) 0.028(2) 0.0230(19) 0.0054(17) 0.0034(17) 0.0017(19) C6 0.045(3) 0.033(3) 0.0233(19) 0.0056(17) 0.0005(17) 0.0004(19) C7 0.040(2) 0.036(3) 0.031(2) -0.0010(19) 0.0009(18) 0.005(2) C8 0.048(3) 0.054(3) 0.037(2) 0.012(2) 0.001(2) 0.002(2) C9 0.045(3) 0.087(4) 0.049(3) 0.016(3) -0.006(2) 0.007(3) C10 0.034(3) 0.093(5) 0.065(3) 0.020(3) -0.006(2) -0.003(3) C11 0.038(3) 0.071(4) 0.058(3) 0.020(3) 0.006(2) -0.002(2) C12 0.042(3) 0.123(6) 0.071(4) 0.048(4) 0.008(3) 0.000(3) C13 0.042(3) 0.167(7) 0.104(5) 0.087(5) -0.001(3) -0.003(4) C14 0.047(3) 0.144(6) 0.078(4) 0.059(4) -0.010(3) 0.005(4) C15 0.054(3) 0.080(4) 0.047(3) 0.026(3) 0.003(2) 0.002(3) C16 0.041(2) 0.044(3) 0.034(2) 0.002(2) 0.0013(18) 0.004(2) C17 0.048(3) 0.033(3) 0.024(2) -0.0031(17) 0.0013(18) -0.002(2) C18 0.051(3) 0.023(2) 0.029(2) 0.0028(17) 0.0092(18) -0.001(2) C19 0.067(3) 0.041(3) 0.027(2) -0.0005(19) 0.008(2) -0.007(2) C20 0.096(4) 0.043(3) 0.026(2) -0.004(2) 0.019(2) -0.007(3) C21 0.087(4) 0.042(3) 0.046(3) -0.003(2) 0.037(3) -0.005(3) C22 0.057(3) 0.043(3) 0.044(2) 0.000(2) 0.020(2) -0.001(2) O 0.114(5) 0.489(17) 0.058(3) 0.015(5) 0.017(3) -0.034(6) N9 0.077(3) 0.047(3) 0.053(3) 0.011(2) 0.019(2) 0.015(2) C23 0.136(9) 0.097(8) 0.46(2) -0.096(12) 0.155(13) -0.011(6) C24 0.166(10) 0.46(2) 0.065(5) 0.040(8) 0.010(6) -0.085(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' Cu Cu 0.3201 1.2651 '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' 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 N5 Cu1 N1 128.65(15) . . ? N5 Cu1 Cu2 80.74(10) . . ? N1 Cu1 Cu2 78.94(9) . . ? N5 Cu1 Br1 106.45(10) . . ? N1 Cu1 Br1 102.03(9) . . ? Cu2 Cu1 Br1 168.91(3) . . ? N5 Cu1 Br2 105.28(10) . 2_656 ? N1 Cu1 Br2 109.90(9) . 2_656 ? Cu2 Cu1 Br2 68.33(2) . 2_656 ? Br1 Cu1 Br2 101.25(3) . 2_656 ? N6 Cu2 N2 157.97(15) . . ? N6 Cu2 Cu1 94.34(10) . . ? N2 Cu2 Cu1 94.60(10) . . ? N6 Cu2 Cu3 86.16(10) . . ? N2 Cu2 Cu3 85.49(10) . . ? Cu1 Cu2 Cu3 178.31(4) . . ? N6 Cu2 Br2 101.08(11) . 2_656 ? N2 Cu2 Br2 100.72(11) . 2_656 ? Cu1 Cu2 Br2 57.72(2) . 2_656 ? Cu3 Cu2 Br2 120.60(3) . 2_656 ? N7 Cu3 N3 169.69(14) . . ? N7 Cu3 Cu2 87.11(10) . . ? N3 Cu3 Cu2 87.85(10) . . ? N7 Cu3 Cu4 92.95(10) . . ? N3 Cu3 Cu4 93.15(10) . . ? Cu2 Cu3 Cu4 172.95(3) . . ? N8 Cu4 N4 139.14(14) . . ? N8 Cu4 Cu3 80.41(9) . . ? N4 Cu4 Cu3 81.64(10) . . ? N8 Cu4 Br1 101.72(10) . 2_646 ? N4 Cu4 Br1 104.12(10) . 2_646 ? Cu3 Cu4 Br1 166.58(3) . 2_646 ? N8 Cu4 Br2 106.66(10) . . ? N4 Cu4 Br2 100.67(10) . . ? Cu3 Cu4 Br2 69.22(2) . . ? Br1 Cu4 Br2 97.61(2) 2_646 . ? Cu1 Br1 Cu4 81.95(2) . 2_656 ? Cu1 Br2 Cu4 78.91(2) 2_646 . ? Cu1 Br2 Cu2 53.957(18) 2_646 2_646 ? Cu4 Br2 Cu2 132.87(2) . 2_646 ? C5 N1 C1 118.2(3) . . ? C5 N1 Cu1 128.5(3) . . ? C1 N1 Cu1 113.2(3) . . ? C6 N2 C5 120.0(3) . . ? C6 N2 Cu2 122.0(3) . . ? C5 N2 Cu2 117.8(3) . . ? C6 N3 C7 120.4(3) . . ? C6 N3 Cu3 119.0(3) . . ? C7 N3 Cu3 119.8(3) . . ? C7 N4 C11 118.1(3) . . ? C7 N4 Cu4 126.7(3) . . ? C11 N4 Cu4 115.0(3) . . ? C16 N5 C12 118.3(4) . . ? C16 N5 Cu1 128.1(3) . . ? C12 N5 Cu1 113.6(3) . . ? C17 N6 C16 119.5(3) . . ? C17 N6 Cu2 121.2(3) . . ? C16 N6 Cu2 119.2(2) . . ? C17 N7 C18 120.8(3) . . ? C17 N7 Cu3 120.4(3) . . ? C18 N7 Cu3 118.7(3) . . ? C18 N8 C22 117.9(3) . . ? C18 N8 Cu4 126.7(3) . . ? C22 N8 Cu4 115.1(3) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C1 C2 C3 117.9(4) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 N2 114.8(3) . . ? N1 C5 C4 120.6(4) . . ? N2 C5 C4 124.5(4) . . ? N2 C6 N3 121.6(3) . . ? N2 C6 H6A 119.2 . . ? N3 C6 H6A 119.2 . . ? N4 C7 N3 116.3(3) . . ? N4 C7 C8 120.5(4) . . ? N3 C7 C8 123.1(4) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 119.8(4) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C9 C10 C11 117.9(4) . . ? C9 C10 H10A 121.0 . . ? C11 C10 H10A 121.0 . . ? N4 C11 C10 123.7(4) . . ? N4 C11 H11A 118.2 . . ? C10 C11 H11A 118.2 . . ? N5 C12 C13 123.2(5) . . ? N5 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C14 C13 C12 117.9(5) . . ? C14 C13 H13A 121.0 . . ? C12 C13 H13A 121.0 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? N5 C16 N6 115.6(3) . . ? N5 C16 C15 120.3(4) . . ? N6 C16 C15 124.1(4) . . ? N6 C17 N7 121.3(3) . . ? N6 C17 H17A 119.4 . . ? N7 C17 H17A 119.4 . . ? N8 C18 N7 115.8(3) . . ? N8 C18 C19 120.9(4) . . ? N7 C18 C19 123.3(4) . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 118.9(4) . . ? C19 C20 H20A 120.5 . . ? C21 C20 H20A 120.5 . . ? C20 C21 C22 118.9(4) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? N8 C22 C21 123.3(4) . . ? N8 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? C25 N9 C23 118.9(10) . . ? C25 N9 C24 115.5(8) . . ? C23 N9 C24 125.2(9) . . ? N9 C23 O 107.5(9) . . ? N9 C23 H23A 126.3 . . ? O C23 H23A 126.3 . . ? N9 C24 H24A 109.5 . . ? N9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 C25 H25A 109.5 . . ? N9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 N5 2.063(3) . ? Cu1 N1 2.064(3) . ? Cu1 Cu2 2.4748(7) . ? Cu1 Br1 2.5623(7) . ? Cu1 Br2 2.5875(7) 2_656 ? Cu2 N6 1.911(3) . ? Cu2 N2 1.912(3) . ? Cu2 Cu3 2.4767(7) . ? Cu2 Br2 2.8443(8) 2_656 ? Cu3 N7 1.902(3) . ? Cu3 N3 1.904(3) . ? Cu3 Cu4 2.4782(7) . ? Cu4 N8 2.034(3) . ? Cu4 N4 2.045(3) . ? Cu4 Br1 2.5764(7) 2_646 ? Cu4 Br2 2.7126(7) . ? Br1 Cu4 2.5764(7) 2_656 ? Br2 Cu1 2.5875(7) 2_646 ? Br2 Cu2 2.8443(8) 2_646 ? N1 C5 1.348(5) . ? N1 C1 1.350(5) . ? N2 C6 1.313(5) . ? N2 C5 1.394(5) . ? N3 C6 1.331(5) . ? N3 C7 1.390(5) . ? N4 C7 1.341(5) . ? N4 C11 1.345(5) . ? N5 C16 1.343(5) . ? N5 C12 1.346(6) . ? N6 C17 1.319(5) . ? N6 C16 1.396(5) . ? N7 C17 1.325(5) . ? N7 C18 1.388(5) . ? N8 C18 1.344(5) . ? N8 C22 1.353(5) . ? C1 C2 1.374(6) . ? C1 H1A 0.9300 . ? C2 C3 1.383(6) . ? C2 H2A 0.9300 . ? C3 C4 1.361(6) . ? C3 H3A 0.9300 . ? C4 C5 1.407(5) . ? C4 H4A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.409(5) . ? C8 C9 1.361(6) . ? C8 H8A 0.9300 . ? C9 C10 1.366(7) . ? C9 H9A 0.9300 . ? C10 C11 1.382(6) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C13 1.381(7) . ? C12 H12A 0.9300 . ? C13 C14 1.354(7) . ? C13 H13A 0.9300 . ? C14 C15 1.356(7) . ? C14 H14A 0.9300 . ? C15 C16 1.400(6) . ? C15 H15A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.413(5) . ? C19 C20 1.370(6) . ? C19 H19A 0.9300 . ? C20 C21 1.370(7) . ? C20 H20A 0.9300 . ? C21 C22 1.384(6) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? O C23 1.383(16) . ? N9 C25 1.293(13) . ? N9 C23 1.319(11) . ? N9 C24 1.392(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ?