#------------------------------------------------------------------------------ #$Date: 2019-06-01 03:26:27 +0300 (Sat, 01 Jun 2019) $ #$Revision: 215644 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/11/1551191.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_1551191 loop_ _publ_author_name 'Fataftah, Majed S.' 'Krzyaniak, Matthew D.' 'Vlaisavljevich, Bess' 'Wasielewski, Michael R.' 'Zadrozny, Joseph' 'Freedman, Danna' _publ_section_title ; Metal-Ligand Covalency Enables Room Temperature Molecular Qubit Candidates ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC00074G _journal_year 2019 _chemical_formula_moiety 'C12 H8 Cu Se4, 2(C24 H20 P)' _chemical_formula_sum 'C60 H48 Cu P2 Se4' _chemical_formula_weight 1210.30 _chemical_name_systematic 'tetraphenyl phosphonium copper bis(diselenocatecholate)' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc210dfx _audit_creation_date 2018-03-27 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-11-05 deposited with the CCDC. 2019-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.517(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.1972(9) _cell_length_b 15.0275(12) _cell_length_c 15.2359(12) _cell_measurement_reflns_used 9827 _cell_measurement_temperature 250.04 _cell_measurement_theta_max 29.89 _cell_measurement_theta_min 2.57 _cell_volume 2555.7(4) _computing_cell_refinement 'SAINT v8.34A (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 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 250.04 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _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 0.0495 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 68791 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.606 _diffrn_reflns_theta_min 1.906 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.378 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.4894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1127 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.6559. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'dull dark red' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.573 _exptl_crystal_description block _exptl_crystal_F_000 1206 _exptl_crystal_preparation 'In DMF, with two equivalents of selenocatechol and 1 equivalent of CuCl2 with NBu4OH and Ph4PBr' _exptl_crystal_recrystallization_method 'Layered DMF solution of the compound under Et2O at -35 C' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.877 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.062 _refine_ls_extinction_coef 0.0028(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 305 _refine_ls_number_reflns 7855 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0303P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.0779 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6612 _reflns_number_total 7855 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc00074g2.cif _cod_data_source_block msf6_49_3 _cod_database_code 1551191 _shelx_shelxl_version_number 2016/6 _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. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C007(H007), C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y) ; _shelx_res_file ; TITL msf6_49_3_a.res in P2(1)/n msf6_49_3.res created by SHELXL-2016/6 at 17:47:34 on 27-Mar-2018 REM Old TITL MSF6_49_3 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.141, Rweak 0.008, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C60 P2 Se5 CELL 0.71073 11.1972 15.0275 15.2359 90 94.517 90 ZERR 2 0.0009 0.0012 0.0012 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cu P Se UNIT 120 96 2 4 8 L.S. 10 PLAN 20 TEMP -23.11 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.030300 1.912300 EXTI 0.002838 FVAR 0.32477 SE01 5 -0.123366 0.482872 0.621855 11.00000 0.04191 0.03754 = 0.03855 0.00989 0.00414 0.00545 SE02 5 0.140175 0.396709 0.566579 11.00000 0.04740 0.04506 = 0.04181 0.01774 0.01017 0.01248 CU03 3 0.000000 0.500000 0.500000 10.50000 0.04000 0.02452 = 0.02855 0.00465 -0.00169 -0.00168 P004 4 0.477247 0.537279 0.796318 11.00000 0.02844 0.02498 = 0.03143 -0.00217 0.00109 0.00143 C005 1 0.601026 0.588645 0.859210 11.00000 0.02639 0.03090 = 0.02948 -0.00001 0.00106 0.00132 C006 1 0.339921 0.572501 0.839500 11.00000 0.02845 0.02575 = 0.04141 -0.00247 0.00323 -0.00024 C007 1 0.611320 0.681308 0.855995 11.00000 0.03054 0.03151 = 0.03879 0.00062 -0.00238 0.00125 AFIX 43 H007 2 0.554691 0.715059 0.821460 11.00000 -1.20000 AFIX 0 C008 1 0.079399 0.371225 0.676133 11.00000 0.04195 0.02488 = 0.02828 0.00431 -0.00523 -0.00670 C009 1 0.486071 0.570883 0.683408 11.00000 0.04414 0.02656 = 0.03080 -0.00126 -0.00218 0.00486 C00A 1 -0.029479 0.406036 0.699032 11.00000 0.04484 0.02640 = 0.02839 0.00361 -0.00271 -0.00726 C00B 1 0.492219 0.418818 0.806078 11.00000 0.03779 0.02563 = 0.03436 -0.00232 0.00194 0.00238 C00C 1 0.146455 0.316846 0.736760 11.00000 0.04846 0.02970 = 0.03861 0.00491 -0.01066 -0.00404 AFIX 43 H00C 2 0.220234 0.293688 0.721978 11.00000 -1.20000 AFIX 0 C00D 1 0.705586 0.723105 0.904069 11.00000 0.03626 0.03818 = 0.04187 -0.00412 0.00244 -0.00754 AFIX 43 H00D 2 0.712001 0.785463 0.903194 11.00000 -1.20000 AFIX 0 C00E 1 0.685871 0.538307 0.908992 11.00000 0.03586 0.03603 = 0.03654 0.00449 -0.00064 0.00545 AFIX 43 H00E 2 0.678991 0.476019 0.911165 11.00000 -1.20000 AFIX 0 C00F 1 0.790070 0.673123 0.953246 11.00000 0.03166 0.05770 = 0.03530 -0.00382 -0.00118 -0.00707 AFIX 43 H00F 2 0.854133 0.701716 0.985381 11.00000 -1.20000 AFIX 0 C00G 1 0.435970 0.372677 0.870336 11.00000 0.05027 0.03264 = 0.04865 0.00033 0.01764 0.00222 AFIX 43 H00G 2 0.382759 0.402453 0.904994 11.00000 -1.20000 AFIX 0 C00H 1 0.595976 0.597763 0.656448 11.00000 0.04792 0.04490 = 0.03655 0.00284 0.00892 0.00829 AFIX 43 H00H 2 0.663798 0.598779 0.696932 11.00000 -1.20000 AFIX 0 C00I 1 0.105709 0.296879 0.817707 11.00000 0.07378 0.03467 = 0.03266 0.00983 -0.01431 -0.00758 AFIX 43 H00I 2 0.151866 0.260793 0.857742 11.00000 -1.20000 AFIX 0 C00J 1 0.341422 0.632844 0.908644 11.00000 0.03443 0.03789 = 0.04134 -0.00772 0.00740 -0.00280 AFIX 43 H00J 2 0.414781 0.654353 0.934518 11.00000 -1.20000 AFIX 0 C00K 1 0.230578 0.539888 0.802415 11.00000 0.03533 0.04247 = 0.06596 -0.01814 0.00200 -0.00638 AFIX 43 H00K 2 0.228899 0.497415 0.757041 11.00000 -1.20000 AFIX 0 C00L 1 -0.002573 0.329936 0.839576 11.00000 0.07868 0.04679 = 0.02877 0.00814 0.00096 -0.01194 AFIX 43 H00L 2 -0.030996 0.315651 0.894272 11.00000 -1.20000 AFIX 0 C00M 1 -0.069996 0.384346 0.781070 11.00000 0.06009 0.04060 = 0.03376 0.00446 0.00673 -0.00472 AFIX 43 H00M 2 -0.143708 0.406909 0.796670 11.00000 -1.20000 AFIX 0 C00N 1 0.458529 0.282345 0.883298 11.00000 0.06487 0.03435 = 0.05586 0.00822 0.01364 0.00023 AFIX 43 H00N 2 0.421344 0.251317 0.927273 11.00000 -1.20000 AFIX 0 C00O 1 0.781176 0.581388 0.955589 11.00000 0.03568 0.05900 = 0.03874 0.00753 -0.00774 0.00675 AFIX 43 H00O 2 0.839624 0.547959 0.988731 11.00000 -1.20000 AFIX 0 C00P 1 0.569562 0.374400 0.754216 11.00000 0.07210 0.03528 = 0.04755 0.00020 0.02585 0.01066 AFIX 43 H00P 2 0.607310 0.404943 0.710205 11.00000 -1.20000 AFIX 0 C00Q 1 0.386666 0.568146 0.622541 11.00000 0.05510 0.04024 = 0.04677 -0.00345 -0.01465 -0.00012 AFIX 43 H00Q 2 0.311930 0.549308 0.639736 11.00000 -1.20000 AFIX 0 C00R 1 0.234624 0.661312 0.939450 11.00000 0.04649 0.04280 = 0.05899 -0.01463 0.01966 -0.00112 AFIX 43 H00R 2 0.235630 0.701518 0.986766 11.00000 -1.20000 AFIX 0 C00S 1 0.605746 0.623083 0.569932 11.00000 0.07574 0.04807 = 0.04281 0.00547 0.02176 0.01340 AFIX 43 H00S 2 0.680234 0.641547 0.551960 11.00000 -1.20000 AFIX 0 C00T 1 0.534857 0.238582 0.832053 11.00000 0.08222 0.02849 = 0.05937 0.00173 0.00881 0.00977 AFIX 43 H00T 2 0.549216 0.177434 0.840517 11.00000 -1.20000 AFIX 0 C00U 1 0.124664 0.570357 0.832740 11.00000 0.03034 0.05628 = 0.08699 -0.01423 0.00451 -0.00853 AFIX 43 H00U 2 0.050884 0.549739 0.806767 11.00000 -1.20000 AFIX 0 C00V 1 0.399262 0.593670 0.535795 11.00000 0.09852 0.04255 = 0.04012 -0.00656 -0.02403 0.01066 AFIX 43 H00V 2 0.332580 0.591808 0.494301 11.00000 -1.20000 AFIX 0 C00W 1 0.126974 0.630727 0.900779 11.00000 0.03510 0.04687 = 0.08570 -0.00389 0.02151 0.00319 AFIX 43 H00W 2 0.054712 0.651219 0.920991 11.00000 -1.20000 AFIX 0 C00X 1 0.507708 0.621397 0.510469 11.00000 0.11060 0.03986 = 0.03179 0.00012 0.00644 0.01704 AFIX 43 H00X 2 0.514864 0.639347 0.452015 11.00000 -1.20000 AFIX 0 C00Y 1 0.590473 0.283842 0.768320 11.00000 0.09844 0.03795 = 0.06810 -0.00153 0.03691 0.02178 AFIX 43 H00Y 2 0.643241 0.253400 0.733820 11.00000 -1.20000 AFIX 0 HKLF 4 REM msf6_49_3_a.res in P2(1)/n REM R1 = 0.0297 for 6612 Fo > 4sig(Fo) and 0.0398 for all 7855 data REM 305 parameters refined using 0 restraints END WGHT 0.0281 1.9890 REM Highest difference peak 0.877, deepest hole -1.072, 1-sigma level 0.062 Q1 1 0.0882 0.3765 0.5474 11.00000 0.05 0.88 Q2 1 -0.1371 0.4539 0.5822 11.00000 0.05 0.70 Q3 1 0.1361 0.4342 0.5673 11.00000 0.05 0.57 Q4 1 -0.0609 0.4947 0.6157 11.00000 0.05 0.50 Q5 1 0.2009 0.3838 0.5567 11.00000 0.05 0.44 Q6 1 0.6613 0.5733 0.8757 11.00000 0.05 0.36 Q7 1 0.4001 0.5585 0.8213 11.00000 0.05 0.35 Q8 1 0.6125 0.6361 0.8597 11.00000 0.05 0.34 Q9 1 -0.0421 0.3874 0.7395 11.00000 0.05 0.32 Q10 1 0.0168 0.3842 0.6875 11.00000 0.05 0.31 Q11 1 0.2897 0.6411 0.9268 11.00000 0.05 0.30 Q12 1 -0.1996 0.4968 0.6283 11.00000 0.05 0.30 Q13 1 0.6621 0.4783 0.6211 11.00000 0.05 0.29 Q14 1 -0.1987 0.4428 0.6397 11.00000 0.05 0.29 Q15 1 0.6006 0.6009 0.6133 11.00000 0.05 0.29 Q16 1 0.4854 0.5551 0.7316 11.00000 0.05 0.28 Q17 1 0.4412 0.5738 0.6491 11.00000 0.05 0.27 Q18 1 -0.1056 0.4980 0.5593 11.00000 0.05 0.27 Q19 1 -0.0824 0.4039 0.5613 11.00000 0.05 0.27 Q20 1 0.4913 0.4743 0.8052 11.00000 0.05 0.27 ; _shelx_res_checksum 7781 _olex2_exptl_crystal_mounting_method 'Mounted under paratone' _olex2_submission_original_sample_id 'Compound 4' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Se01 Se -0.12337(2) 0.48287(2) 0.62185(2) 0.03928(6) Uani 1 1 d . . . Se02 Se 0.14017(2) 0.39671(2) 0.56658(2) 0.04440(7) Uani 1 1 d . . . Cu03 Cu 0.000000 0.500000 0.500000 0.03125(8) Uani 1 2 d S T P P004 P 0.47725(4) 0.53728(3) 0.79632(3) 0.02835(9) Uani 1 1 d . . . C005 C 0.60103(15) 0.58864(12) 0.85921(11) 0.0290(3) Uani 1 1 d . . . C006 C 0.33992(16) 0.57250(12) 0.83950(13) 0.0318(3) Uani 1 1 d . . . C007 C 0.61132(17) 0.68131(13) 0.85599(13) 0.0339(4) Uani 1 1 d . . . H007 H 0.554691 0.715059 0.821460 0.041 Uiso 1 1 calc R . . C008 C 0.07940(18) 0.37123(12) 0.67613(12) 0.0321(4) Uani 1 1 d . . . C009 C 0.48607(18) 0.57088(12) 0.68341(12) 0.0341(4) Uani 1 1 d . . . C00A C -0.02948(18) 0.40604(12) 0.69903(12) 0.0335(4) Uani 1 1 d . . . C00B C 0.49222(17) 0.41882(12) 0.80608(12) 0.0326(4) Uani 1 1 d . . . C00C C 0.1465(2) 0.31685(13) 0.73676(13) 0.0397(4) Uani 1 1 d . . . H00C H 0.220234 0.293688 0.721978 0.048 Uiso 1 1 calc R . . C00D C 0.70559(18) 0.72311(14) 0.90407(13) 0.0388(4) Uani 1 1 d . . . H00D H 0.712001 0.785463 0.903194 0.047 Uiso 1 1 calc R . . C00E C 0.68587(18) 0.53831(14) 0.90899(13) 0.0363(4) Uani 1 1 d . . . H00E H 0.678991 0.476019 0.911165 0.044 Uiso 1 1 calc R . . C00F C 0.79007(18) 0.67312(16) 0.95325(13) 0.0418(5) Uani 1 1 d . . . H00F H 0.854133 0.701716 0.985381 0.050 Uiso 1 1 calc R . . C00G C 0.4360(2) 0.37268(14) 0.87034(15) 0.0431(5) Uani 1 1 d . . . H00G H 0.382759 0.402453 0.904994 0.052 Uiso 1 1 calc R . . C00H C 0.5960(2) 0.59776(15) 0.65645(14) 0.0428(5) Uani 1 1 d . . . H00H H 0.663798 0.598779 0.696932 0.051 Uiso 1 1 calc R . . C00I C 0.1057(2) 0.29688(14) 0.81771(14) 0.0480(5) Uani 1 1 d . . . H00I H 0.151866 0.260793 0.857742 0.058 Uiso 1 1 calc R . . C00J C 0.34142(18) 0.63284(14) 0.90864(14) 0.0377(4) Uani 1 1 d . . . H00J H 0.414781 0.654353 0.934518 0.045 Uiso 1 1 calc R . . C00K C 0.2306(2) 0.53989(15) 0.80241(17) 0.0480(5) Uani 1 1 d . . . H00K H 0.228899 0.497415 0.757041 0.058 Uiso 1 1 calc R . . C00L C -0.0026(3) 0.32994(16) 0.83958(14) 0.0516(6) Uani 1 1 d . . . H00L H -0.030996 0.315651 0.894272 0.062 Uiso 1 1 calc R . . C00M C -0.0700(2) 0.38435(15) 0.78107(14) 0.0447(5) Uani 1 1 d . . . H00M H -0.143708 0.406909 0.796670 0.054 Uiso 1 1 calc R . . C00N C 0.4585(2) 0.28234(15) 0.88330(17) 0.0512(5) Uani 1 1 d . . . H00N H 0.421344 0.251317 0.927273 0.061 Uiso 1 1 calc R . . C00O C 0.78118(19) 0.58139(17) 0.95559(14) 0.0450(5) Uani 1 1 d . . . H00O H 0.839624 0.547959 0.988731 0.054 Uiso 1 1 calc R . . C00P C 0.5696(2) 0.37440(15) 0.75422(16) 0.0505(6) Uani 1 1 d . . . H00P H 0.607310 0.404943 0.710205 0.061 Uiso 1 1 calc R . . C00Q C 0.3867(2) 0.56815(15) 0.62254(15) 0.0484(5) Uani 1 1 d . . . H00Q H 0.311930 0.549308 0.639736 0.058 Uiso 1 1 calc R . . C00R C 0.2346(2) 0.66131(15) 0.93945(17) 0.0486(5) Uani 1 1 d . . . H00R H 0.235630 0.701518 0.986766 0.058 Uiso 1 1 calc R . . C00S C 0.6057(3) 0.62308(17) 0.56993(16) 0.0546(6) Uani 1 1 d . . . H00S H 0.680234 0.641547 0.551960 0.066 Uiso 1 1 calc R . . C00T C 0.5349(3) 0.23858(15) 0.83205(17) 0.0565(6) Uani 1 1 d . . . H00T H 0.549216 0.177434 0.840517 0.068 Uiso 1 1 calc R . . C00U C 0.1247(2) 0.57036(18) 0.8327(2) 0.0579(7) Uani 1 1 d . . . H00U H 0.050884 0.549739 0.806767 0.069 Uiso 1 1 calc R . . C00V C 0.3993(3) 0.59367(17) 0.53579(17) 0.0620(8) Uani 1 1 d . . . H00V H 0.332580 0.591808 0.494301 0.074 Uiso 1 1 calc R . . C00W C 0.1270(2) 0.63073(17) 0.9008(2) 0.0550(6) Uani 1 1 d . . . H00W H 0.054712 0.651219 0.920991 0.066 Uiso 1 1 calc R . . C00X C 0.5077(3) 0.62140(16) 0.51047(15) 0.0607(8) Uani 1 1 d . . . H00X H 0.514864 0.639347 0.452015 0.073 Uiso 1 1 calc R . . C00Y C 0.5905(3) 0.28384(17) 0.76832(19) 0.0666(8) Uani 1 1 d . . . H00Y H 0.643241 0.253400 0.733820 0.080 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 Se01 0.04191(12) 0.03754(11) 0.03855(11) 0.00989(8) 0.00414(8) 0.00545(8) Se02 0.04740(13) 0.04506(12) 0.04181(12) 0.01774(9) 0.01017(9) 0.01248(9) Cu03 0.04000(17) 0.02452(14) 0.02855(15) 0.00465(11) -0.00169(12) -0.00168(12) P004 0.0284(2) 0.02498(19) 0.0314(2) -0.00217(16) 0.00109(16) 0.00143(16) C005 0.0264(8) 0.0309(8) 0.0295(8) 0.0000(6) 0.0011(6) 0.0013(6) C006 0.0284(8) 0.0258(8) 0.0414(9) -0.0025(7) 0.0032(7) -0.0002(6) C007 0.0305(9) 0.0315(8) 0.0388(9) 0.0006(7) -0.0024(7) 0.0013(7) C008 0.0420(10) 0.0249(7) 0.0283(8) 0.0043(6) -0.0052(7) -0.0067(7) C009 0.0441(10) 0.0266(8) 0.0308(8) -0.0013(6) -0.0022(7) 0.0049(7) C00A 0.0448(10) 0.0264(8) 0.0284(8) 0.0036(6) -0.0027(7) -0.0073(7) C00B 0.0378(9) 0.0256(8) 0.0344(9) -0.0023(7) 0.0019(7) 0.0024(7) C00C 0.0485(11) 0.0297(9) 0.0386(10) 0.0049(7) -0.0107(8) -0.0040(8) C00D 0.0363(10) 0.0382(10) 0.0419(10) -0.0041(8) 0.0024(8) -0.0075(8) C00E 0.0359(10) 0.0360(9) 0.0365(9) 0.0045(7) -0.0006(7) 0.0054(7) C00F 0.0317(10) 0.0577(13) 0.0353(9) -0.0038(9) -0.0012(7) -0.0071(9) C00G 0.0503(12) 0.0326(9) 0.0487(11) 0.0003(8) 0.0176(9) 0.0022(8) C00H 0.0479(12) 0.0449(11) 0.0366(10) 0.0028(8) 0.0089(8) 0.0083(9) C00I 0.0738(16) 0.0347(10) 0.0327(10) 0.0098(8) -0.0143(10) -0.0076(10) C00J 0.0344(9) 0.0379(10) 0.0413(10) -0.0077(8) 0.0074(8) -0.0028(8) C00K 0.0353(10) 0.0425(11) 0.0660(14) -0.0181(10) 0.0020(10) -0.0064(9) C00L 0.0787(17) 0.0468(12) 0.0288(9) 0.0081(8) 0.0010(10) -0.0119(12) C00M 0.0601(14) 0.0406(10) 0.0338(10) 0.0045(8) 0.0067(9) -0.0047(9) C00N 0.0649(15) 0.0344(10) 0.0559(13) 0.0082(9) 0.0136(11) 0.0002(10) C00O 0.0357(10) 0.0590(13) 0.0387(10) 0.0075(9) -0.0077(8) 0.0067(9) C00P 0.0721(16) 0.0353(10) 0.0475(12) 0.0002(9) 0.0259(11) 0.0107(10) C00Q 0.0551(13) 0.0402(11) 0.0468(12) -0.0035(9) -0.0147(10) -0.0001(9) C00R 0.0465(12) 0.0428(11) 0.0590(13) -0.0146(10) 0.0197(10) -0.0011(9) C00S 0.0757(17) 0.0481(12) 0.0428(12) 0.0055(10) 0.0218(11) 0.0134(12) C00T 0.0822(18) 0.0285(10) 0.0594(14) 0.0017(9) 0.0088(13) 0.0098(11) C00U 0.0303(11) 0.0563(14) 0.0870(19) -0.0142(13) 0.0045(11) -0.0085(10) C00V 0.099(2) 0.0425(12) 0.0401(12) -0.0066(10) -0.0240(13) 0.0107(13) C00W 0.0351(11) 0.0469(12) 0.0857(18) -0.0039(12) 0.0215(11) 0.0032(9) C00X 0.111(2) 0.0399(11) 0.0318(10) 0.0001(9) 0.0064(12) 0.0170(13) C00Y 0.098(2) 0.0380(12) 0.0681(17) -0.0015(11) 0.0369(16) 0.0218(13) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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 C00A Se01 Cu03 102.60(6) . . C008 Se02 Cu03 103.74(6) . . Se01 Cu03 Se01 180.0 . 3_566 Se02 Cu03 Se01 90.044(9) 3_566 3_566 Se02 Cu03 Se01 90.044(8) . . Se02 Cu03 Se01 89.956(8) . 3_566 Se02 Cu03 Se01 89.955(8) 3_566 . Se02 Cu03 Se02 180.0 3_566 . C005 P004 C006 108.92(8) . . C005 P004 C009 106.90(9) . . C006 P004 C009 112.28(9) . . C00B P004 C005 108.62(9) . . C00B P004 C006 109.80(9) . . C00B P004 C009 110.20(9) . . C007 C005 P004 118.13(13) . . C00E C005 P004 121.48(15) . . C00E C005 C007 120.38(17) . . C00J C006 P004 120.65(14) . . C00J C006 C00K 119.60(18) . . C00K C006 P004 119.75(15) . . C005 C007 H007 120.2 . . C00D C007 C005 119.60(18) . . C00D C007 H007 120.2 . . C00A C008 Se02 121.80(13) . . C00A C008 C00C 119.04(18) . . C00C C008 Se02 119.15(16) . . C00H C009 P004 118.71(15) . . C00H C009 C00Q 119.5(2) . . C00Q C009 P004 121.76(17) . . C008 C00A Se01 121.56(13) . . C008 C00A C00M 119.09(18) . . C00M C00A Se01 119.34(17) . . C00G C00B P004 120.59(15) . . C00P C00B P004 119.24(16) . . C00P C00B C00G 119.90(18) . . C008 C00C H00C 119.5 . . C00I C00C C008 121.1(2) . . C00I C00C H00C 119.5 . . C007 C00D H00D 120.0 . . C00F C00D C007 120.0(2) . . C00F C00D H00D 120.0 . . C005 C00E H00E 120.4 . . C005 C00E C00O 119.18(19) . . C00O C00E H00E 120.4 . . C00D C00F H00F 119.7 . . C00D C00F C00O 120.55(19) . . C00O C00F H00F 119.7 . . C00B C00G H00G 120.0 . . C00B C00G C00N 119.9(2) . . C00N C00G H00G 120.0 . . C009 C00H H00H 120.0 . . C00S C00H C009 120.0(2) . . C00S C00H H00H 120.0 . . C00C C00I H00I 120.1 . . C00L C00I C00C 119.8(2) . . C00L C00I H00I 120.1 . . C006 C00J H00J 120.0 . . C00R C00J C006 119.9(2) . . C00R C00J H00J 120.0 . . C006 C00K H00K 120.1 . . C00U C00K C006 119.7(2) . . C00U C00K H00K 120.1 . . C00I C00L H00L 119.9 . . C00I C00L C00M 120.2(2) . . C00M C00L H00L 119.9 . . C00A C00M H00M 119.6 . . C00L C00M C00A 120.8(2) . . C00L C00M H00M 119.6 . . C00G C00N H00N 119.9 . . C00T C00N C00G 120.1(2) . . C00T C00N H00N 119.9 . . C00E C00O H00O 119.9 . . C00F C00O C00E 120.25(19) . . C00F C00O H00O 119.9 . . C00B C00P H00P 120.5 . . C00B C00P C00Y 119.1(2) . . C00Y C00P H00P 120.5 . . C009 C00Q H00Q 120.4 . . C009 C00Q C00V 119.2(3) . . C00V C00Q H00Q 120.4 . . C00J C00R H00R 120.0 . . C00W C00R C00J 120.1(2) . . C00W C00R H00R 120.0 . . C00H C00S H00S 119.8 . . C00X C00S C00H 120.4(3) . . C00X C00S H00S 119.8 . . C00N C00T H00T 119.9 . . C00N C00T C00Y 120.2(2) . . C00Y C00T H00T 119.9 . . C00K C00U H00U 119.9 . . C00W C00U C00K 120.2(2) . . C00W C00U H00U 119.9 . . C00Q C00V H00V 119.7 . . C00X C00V C00Q 120.6(2) . . C00X C00V H00V 119.7 . . C00R C00W H00W 119.8 . . C00U C00W C00R 120.4(2) . . C00U C00W H00W 119.8 . . C00S C00X H00X 119.9 . . C00V C00X C00S 120.2(2) . . C00V C00X H00X 119.9 . . C00P C00Y H00Y 119.6 . . C00T C00Y C00P 120.8(2) . . C00T C00Y H00Y 119.6 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se01 Cu03 2.4135(2) Se01 C00A 1.9043(19) Se02 Cu03 2.3772(2) Se02 C008 1.8907(19) P004 C005 1.7960(18) P004 C006 1.7991(19) P004 C009 1.8030(19) P004 C00B 1.7931(18) C005 C007 1.398(3) C005 C00E 1.392(2) C006 C00J 1.389(3) C006 C00K 1.396(3) C007 H007 0.9400 C007 C00D 1.387(3) C008 C00A 1.396(3) C008 C00C 1.406(3) C009 C00H 1.388(3) C009 C00Q 1.392(3) C00A C00M 1.401(3) C00B C00G 1.390(3) C00B C00P 1.388(3) C00C H00C 0.9400 C00C C00I 1.381(3) C00D H00D 0.9400 C00D C00F 1.382(3) C00E H00E 0.9400 C00E C00O 1.394(3) C00F H00F 0.9400 C00F C00O 1.383(3) C00G H00G 0.9400 C00G C00N 1.392(3) C00H H00H 0.9400 C00H C00S 1.385(3) C00I H00I 0.9400 C00I C00L 1.375(4) C00J H00J 0.9400 C00J C00R 1.386(3) C00K H00K 0.9400 C00K C00U 1.384(3) C00L H00L 0.9400 C00L C00M 1.388(3) C00M H00M 0.9400 C00N H00N 0.9400 C00N C00T 1.370(4) C00O H00O 0.9400 C00P H00P 0.9400 C00P C00Y 1.395(3) C00Q H00Q 0.9400 C00Q C00V 1.394(4) C00R H00R 0.9400 C00R C00W 1.378(4) C00S H00S 0.9400 C00S C00X 1.367(4) C00T H00T 0.9400 C00T C00Y 1.374(4) C00U H00U 0.9400 C00U C00W 1.376(4) C00V H00V 0.9400 C00V C00X 1.368(5) C00W H00W 0.9400 C00X H00X 0.9400 C00Y H00Y 0.9400