#------------------------------------------------------------------------------ #$Date: 2017-09-14 05:44:07 +0300 (Thu, 14 Sep 2017) $ #$Revision: 200875 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044222.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_7044222 loop_ _publ_author_name 'Schmid, Paul' 'Maier, Matthias' 'Pfeiffer, Hendrik' 'Belz, Anja' 'Henry, Lucas' 'Friedrich, Alexandra' 'Sch\"onfeld, Fabian' 'Edkins, Katharina' 'Schatzschneider, Ulrich' _publ_section_title ; Catalyst-free room-temperature iClick reaction of molybdenum(II) and tungsten(II) azide complexes with electron-poor alkynes: Structural preferences and kinetic studies ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT03096G _journal_year 2017 _chemical_formula_moiety 'C21 H18 F3 Mo N5 O4' _chemical_formula_sum 'C21 H18 F3 Mo N5 O4' _chemical_formula_weight 557.34 _chemical_name_common '[Mo(allyl)(triazolateCF3,COOEt)(bpy)(CO)2]' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2012-12-14 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-07-17 deposited with the CCDC. 2017-09-13 downloaded from the CCDC. ; _cell_angle_alpha 82.745(7) _cell_angle_beta 63.061(8) _cell_angle_gamma 75.89(2) _cell_formula_units_Z 2 _cell_length_a 10.545(2) _cell_length_b 10.8506(19) _cell_length_c 11.320(2) _cell_measurement_reflns_used 4160 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 22.67 _cell_measurement_theta_min 2.25 _cell_volume 1119.7(4) _computing_cell_refinement 'Saint+ ver. V8.18C (Bruker AXS)' _computing_data_reduction 'Saint+ ver. V8.18C (Bruker AXS)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 273(2) _diffrn_detector 'CCD area detector (Apex2)' _diffrn_detector_area_resol_mean 8.333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker X8-APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0480 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 15715 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.843 _diffrn_reflns_theta_min 2.216 _diffrn_source 'rotating-anode (Nonius FR-591)' _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_correction_T_min 0.8842 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details 'SadAbs 2008/1 (Bruker AXS)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.653 _exptl_crystal_description prism _exptl_crystal_F_000 560 _exptl_crystal_preparation 'prepared dry' _exptl_crystal_recrystallization_method 'by precipitation with hexane from a DCM solution' _exptl_crystal_size_max 0.454 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.085 _refine_diff_density_max 0.368 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 323 _refine_ls_number_reflns 4788 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0330 _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^)+(0.0278P)^2^+0.2457P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.0679 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3932 _reflns_number_total 4788 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt03096g2.cif _cod_data_source_block 12s039_pl _cod_database_code 7044222 _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_res_file ; 12s039_pl.res created by SHELXL-2014/7 TITL 12S039 P 1 R = 0.04 New: P-1 REM estimated errors from Monte Carlo simulation using 16 cycles CELL 0.71073 10.5455 10.8506 11.3204 82.745 63.061 75.889 ZERR 2 0.0020 0.0019 0.0024 0.007 0.008 0.020 REM CELL 0.71073 10.5455 10.8506 11.3204 82.745 63.061 75.889 REM ZERR 2 0.0010 0.0010 0.0010 0.003 0.003 0.003 LATT 1 SFAC C H F Mo N O UNIT 42 36 6 2 10 8 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 0 L.S. 5 FMAP 2 PLAN -20 ACTA BOND $H CONF DFIX 0.95 0.005 C15 H15A C15 H15B C16 H16 C17 H17A C17 H17B WGHT 0.027800 0.245700 FVAR 0.16691 MO1 4 0.136113 -0.216809 0.181212 11.00000 0.02473 0.02512 = 0.02556 0.00103 -0.01113 -0.00460 F1 3 0.323098 -0.068652 0.530766 11.00000 0.09625 0.12725 = 0.13319 -0.09668 -0.07296 0.03815 F2 3 0.546941 -0.151977 0.447076 11.00000 0.06387 0.09969 = 0.09308 -0.02988 -0.03921 -0.03165 F3 3 0.398120 -0.256148 0.585202 11.00000 0.14923 0.15224 = 0.05359 0.01784 -0.06131 -0.08201 O1 6 0.150447 -0.506437 0.239464 11.00000 0.06106 0.02723 = 0.08333 0.00995 -0.04149 -0.01055 O2 6 -0.089503 -0.209398 0.478122 11.00000 0.05204 0.08938 = 0.03305 0.00549 -0.00229 -0.01296 O3 6 0.711152 -0.463231 0.158786 11.00000 0.04757 0.08233 = 0.05369 -0.02622 -0.02639 0.01848 O4 6 0.659366 -0.419267 0.365419 11.00000 0.03857 0.05431 = 0.04511 -0.00391 -0.02596 0.00333 N1 5 0.427759 -0.325851 0.206531 11.00000 0.02962 0.03521 = 0.03217 0.00007 -0.01614 -0.00602 N2 5 0.304972 -0.238276 0.251283 11.00000 0.03083 0.03008 = 0.03178 -0.00020 -0.01548 -0.00554 N3 5 0.285090 -0.174723 0.354526 11.00000 0.03639 0.03537 = 0.03974 -0.00834 -0.01837 -0.00403 N4 5 0.328898 -0.214105 -0.012552 11.00000 0.03010 0.04130 = 0.02684 -0.00338 -0.01305 -0.00449 N5 5 0.169888 -0.017479 0.144264 11.00000 0.03756 0.02599 = 0.03732 0.00011 -0.01919 -0.00359 C1 1 0.144992 -0.399034 0.215618 11.00000 0.03169 0.03802 = 0.04385 0.00021 -0.02141 -0.00692 C2 1 -0.007730 -0.210299 0.368010 11.00000 0.03632 0.04086 = 0.03782 0.00448 -0.01625 -0.00619 C3 1 0.402507 -0.225588 0.375945 11.00000 0.03295 0.03670 = 0.03650 -0.00273 -0.01742 -0.01014 C4 1 0.491689 -0.319826 0.284128 11.00000 0.03003 0.03199 = 0.03118 0.00132 -0.01425 -0.00886 C5 1 0.411941 -0.319327 -0.083789 11.00000 0.03848 0.05775 = 0.03727 -0.01377 -0.01711 0.00324 AFIX 43 H5 2 0.386399 -0.397036 -0.050251 11.00000 -1.20000 AFIX 0 C6 1 0.530987 -0.317481 -0.202037 11.00000 0.03952 0.10318 = 0.04249 -0.02502 -0.01561 0.00335 AFIX 43 H6 2 0.585098 -0.392017 -0.248269 11.00000 -1.20000 AFIX 0 C7 1 0.568892 -0.204301 -0.250916 11.00000 0.03392 0.14012 = 0.02822 -0.01345 -0.00286 -0.01559 AFIX 43 H7 2 0.648892 -0.200450 -0.332251 11.00000 -1.20000 AFIX 0 C8 1 0.488966 -0.095173 -0.180150 11.00000 0.05059 0.09245 = 0.04110 0.01874 -0.02132 -0.03528 AFIX 43 H8 2 0.515493 -0.017667 -0.212883 11.00000 -1.20000 AFIX 0 C9 1 0.367994 -0.101515 -0.059095 11.00000 0.03058 0.05809 = 0.02871 0.00699 -0.01631 -0.01701 C10 1 0.278994 0.007735 0.027738 11.00000 0.04349 0.04038 = 0.03867 0.01258 -0.02770 -0.01830 C11 1 0.306552 0.128420 -0.005108 11.00000 0.08093 0.05274 = 0.06148 0.02221 -0.04600 -0.03674 AFIX 43 H11 2 0.381500 0.144003 -0.086231 11.00000 -1.20000 AFIX 0 C12 1 0.223382 0.225100 0.081919 11.00000 0.11148 0.03872 = 0.09166 0.02147 -0.07544 -0.03258 AFIX 43 H12 2 0.239413 0.307247 0.059530 11.00000 -1.20000 AFIX 0 C13 1 0.116825 0.199707 0.201734 11.00000 0.08812 0.03138 = 0.08498 -0.01398 -0.06005 0.00261 AFIX 43 H13 2 0.061466 0.263728 0.263292 11.00000 -1.20000 AFIX 0 C14 1 0.091761 0.077490 0.230954 11.00000 0.05538 0.03438 = 0.05382 -0.00879 -0.03049 0.00141 AFIX 43 H14 2 0.018822 0.060539 0.312862 11.00000 -1.20000 AFIX 0 C15 1 0.052391 -0.295573 0.053487 11.00000 0.04091 0.04505 = 0.05323 -0.00449 -0.03046 -0.00789 H15A 2 0.129932 -0.334772 -0.024250 11.00000 -1.20000 H15B 2 -0.017816 -0.344358 0.107585 11.00000 -1.20000 C16 1 0.006188 -0.163601 0.067261 11.00000 0.03651 0.04059 = 0.04098 0.00325 -0.02412 -0.00599 H16 2 0.048597 -0.106327 -0.002562 11.00000 -1.20000 C17 1 -0.092627 -0.119847 0.194115 11.00000 0.03084 0.04822 = 0.04773 -0.00034 -0.02033 0.00019 H17A 2 -0.162664 -0.168215 0.249455 11.00000 -1.20000 H17B 2 -0.116988 -0.032633 0.215283 11.00000 -1.20000 C18 1 0.417473 -0.174941 0.483586 11.00000 0.04853 0.06523 = 0.05331 -0.01898 -0.02454 -0.00667 C19 1 0.632085 -0.407895 0.260036 11.00000 0.03560 0.03805 = 0.04187 -0.00051 -0.01980 -0.00719 C20 1 0.792198 -0.508451 0.353551 11.00000 0.03671 0.06251 = 0.05434 0.00248 -0.02428 0.00277 AFIX 23 H20A 2 0.876047 -0.483094 0.280404 11.00000 -1.20000 H20B 2 0.789356 -0.593045 0.336940 11.00000 -1.20000 AFIX 0 C21 1 0.802681 -0.508060 0.479079 11.00000 0.04960 0.06408 = 0.05360 0.01212 -0.02934 -0.01068 AFIX 137 H21A 2 0.806088 -0.424116 0.494265 11.00000 -1.50000 H21B 2 0.889498 -0.566509 0.473919 11.00000 -1.50000 H21C 2 0.719280 -0.533302 0.550752 11.00000 -1.50000 AFIX 0 HKLF 4 REM 12S039 P 1 R = 0.04 New: P-1 REM R1 = 0.0330 for 3932 Fo > 4sig(Fo) and 0.0476 for all 4788 data REM 323 parameters refined using 5 restraints END WGHT 0.0281 0.2210 REM Highest difference peak 0.368, deepest hole -0.407, 1-sigma level 0.069 Q1 1 0.2728 -0.1648 0.5879 11.00000 0.05 0.37 Q2 1 0.4162 -0.3201 0.5856 11.00000 0.05 0.33 Q3 1 0.3823 -0.1077 -0.1224 11.00000 0.05 0.29 Q4 1 0.1017 -0.2329 0.2927 11.00000 0.05 0.28 Q5 1 0.5425 -0.2421 -0.2099 11.00000 0.05 0.28 Q6 1 0.0284 -0.1872 0.2768 11.00000 0.05 0.27 Q7 1 0.4752 -0.0210 -0.1580 11.00000 0.05 0.27 Q8 1 0.3425 -0.2571 -0.0607 11.00000 0.05 0.27 Q9 1 0.5779 -0.3331 0.2620 11.00000 0.05 0.27 Q10 1 0.4647 -0.2429 0.3130 11.00000 0.05 0.26 Q11 1 0.4322 -0.2957 0.3574 11.00000 0.05 0.26 Q12 1 0.0391 0.2253 0.2616 11.00000 0.05 0.25 Q13 1 0.0980 0.9434 0.4536 11.00000 0.05 0.25 Q14 1 0.3953 -0.4401 0.2010 11.00000 0.05 0.25 Q15 1 0.5747 -0.1159 -0.2406 11.00000 0.05 0.25 Q16 1 0.0631 -0.2718 0.2179 11.00000 0.05 0.24 Q17 1 0.5043 0.0595 -0.1832 11.00000 0.05 0.24 Q18 1 0.8291 -0.5994 0.5172 11.00000 0.05 0.23 Q19 1 0.4802 -0.3175 0.2378 11.00000 0.05 0.23 Q20 1 0.3368 -0.0429 0.4852 11.00000 0.05 0.23 ; _shelx_res_checksum 37323 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 Mo1 Mo 0.13611(2) -0.21681(2) 0.18121(2) 0.02537(7) Uani 1 1 d . . F1 F 0.3231(3) -0.0687(3) 0.5308(3) 0.1128(10) Uani 1 1 d . . F2 F 0.5469(2) -0.1520(2) 0.4471(2) 0.0782(6) Uani 1 1 d . . F3 F 0.3981(3) -0.2561(3) 0.5852(2) 0.1041(9) Uani 1 1 d . . O1 O 0.1504(2) -0.50644(18) 0.2395(2) 0.0542(6) Uani 1 1 d . . O2 O -0.0895(2) -0.2094(2) 0.4781(2) 0.0655(7) Uani 1 1 d . . O3 O 0.7112(2) -0.4632(2) 0.1588(2) 0.0633(7) Uani 1 1 d . . O4 O 0.6594(2) -0.41927(19) 0.36542(19) 0.0453(5) Uani 1 1 d . . N1 N 0.4278(2) -0.3259(2) 0.2065(2) 0.0316(5) Uani 1 1 d . . N2 N 0.3050(2) -0.2383(2) 0.2513(2) 0.0304(5) Uani 1 1 d . . N3 N 0.2851(2) -0.1747(2) 0.3545(2) 0.0365(5) Uani 1 1 d . . N4 N 0.3289(2) -0.2141(2) -0.0126(2) 0.0328(5) Uani 1 1 d . . N5 N 0.1699(2) -0.0175(2) 0.1443(2) 0.0332(5) Uani 1 1 d . . C1 C 0.1450(3) -0.3990(3) 0.2156(3) 0.0361(6) Uani 1 1 d . . C2 C -0.0077(3) -0.2103(3) 0.3680(3) 0.0392(7) Uani 1 1 d . . C3 C 0.4025(3) -0.2256(3) 0.3759(3) 0.0338(6) Uani 1 1 d . . C4 C 0.4917(3) -0.3198(2) 0.2841(3) 0.0305(6) Uani 1 1 d . . C5 C 0.4119(3) -0.3193(3) -0.0838(3) 0.0456(8) Uani 1 1 d . . H5 H 0.3864 -0.3970 -0.0503 0.055 Uiso 1 1 calc R U C6 C 0.5310(4) -0.3175(4) -0.2020(3) 0.0639(10) Uani 1 1 d . . H6 H 0.5851 -0.3920 -0.2483 0.077 Uiso 1 1 calc R U C7 C 0.5689(4) -0.2043(5) -0.2509(3) 0.0710(12) Uani 1 1 d . . H7 H 0.6489 -0.2004 -0.3323 0.085 Uiso 1 1 calc R U C8 C 0.4890(4) -0.0952(4) -0.1801(3) 0.0590(10) Uani 1 1 d . . H8 H 0.5155 -0.0177 -0.2129 0.071 Uiso 1 1 calc R U C9 C 0.3680(3) -0.1015(3) -0.0591(3) 0.0371(7) Uani 1 1 d . . C10 C 0.2790(3) 0.0077(3) 0.0277(3) 0.0366(7) Uani 1 1 d . . C11 C 0.3066(4) 0.1284(3) -0.0051(4) 0.0572(9) Uani 1 1 d . . H11 H 0.3815 0.1440 -0.0862 0.069 Uiso 1 1 calc R U C12 C 0.2234(5) 0.2251(3) 0.0819(4) 0.0676(11) Uani 1 1 d . . H12 H 0.2394 0.3072 0.0595 0.081 Uiso 1 1 calc R U C13 C 0.1168(4) 0.1997(3) 0.2017(4) 0.0612(10) Uani 1 1 d . . H13 H 0.0615 0.2637 0.2633 0.073 Uiso 1 1 calc R U C14 C 0.0918(3) 0.0775(3) 0.2310(3) 0.0466(8) Uani 1 1 d . . H14 H 0.0188 0.0605 0.3129 0.056 Uiso 1 1 calc R U C15 C 0.0524(3) -0.2956(3) 0.0535(3) 0.0425(7) Uani 1 1 d D . H15A H 0.130(2) -0.335(2) -0.0242(16) 0.051 Uiso 1 1 d D U H15B H -0.018(2) -0.344(2) 0.108(2) 0.051 Uiso 1 1 d D U C16 C 0.0062(3) -0.1636(3) 0.0673(3) 0.0374(7) Uani 1 1 d D . H16 H 0.049(3) -0.106(2) -0.0026(19) 0.045 Uiso 1 1 d D U C17 C -0.0926(3) -0.1198(3) 0.1941(3) 0.0428(7) Uani 1 1 d D . H17A H -0.163(2) -0.168(2) 0.249(2) 0.051 Uiso 1 1 d D U H17B H -0.117(3) -0.0326(9) 0.215(3) 0.051 Uiso 1 1 d D U C18 C 0.4175(4) -0.1749(3) 0.4836(3) 0.0541(8) Uani 1 1 d . . C19 C 0.6321(3) -0.4079(3) 0.2600(3) 0.0376(6) Uani 1 1 d . . C20 C 0.7922(3) -0.5085(3) 0.3536(3) 0.0524(8) Uani 1 1 d . . H20A H 0.8760 -0.4831 0.2804 0.063 Uiso 1 1 calc R U H20B H 0.7894 -0.5930 0.3369 0.063 Uiso 1 1 calc R U C21 C 0.8027(3) -0.5081(3) 0.4791(3) 0.0547(9) Uani 1 1 d . . H21A H 0.8061 -0.4241 0.4943 0.082 Uiso 1 1 calc R U H21B H 0.8895 -0.5665 0.4739 0.082 Uiso 1 1 calc R U H21C H 0.7193 -0.5333 0.5508 0.082 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 Mo1 0.02473(12) 0.02512(12) 0.02556(12) 0.00103(8) -0.01113(9) -0.00460(8) F1 0.0963(18) 0.127(2) 0.133(2) -0.0967(19) -0.0730(17) 0.0382(16) F2 0.0639(13) 0.0997(17) 0.0931(16) -0.0299(13) -0.0392(12) -0.0317(12) F3 0.149(2) 0.152(2) 0.0536(13) 0.0178(15) -0.0613(15) -0.082(2) O1 0.0611(14) 0.0272(11) 0.0833(17) 0.0100(11) -0.0415(13) -0.0105(10) O2 0.0520(14) 0.0894(18) 0.0330(12) 0.0055(12) -0.0023(11) -0.0130(13) O3 0.0476(14) 0.0823(18) 0.0537(14) -0.0262(13) -0.0264(12) 0.0185(12) O4 0.0386(11) 0.0543(13) 0.0451(12) -0.0039(10) -0.0260(10) 0.0033(9) N1 0.0296(12) 0.0352(13) 0.0322(12) 0.0001(10) -0.0161(10) -0.0060(10) N2 0.0308(12) 0.0301(12) 0.0318(12) -0.0002(10) -0.0155(10) -0.0055(9) N3 0.0364(13) 0.0354(13) 0.0397(13) -0.0083(11) -0.0184(11) -0.0040(10) N4 0.0301(12) 0.0413(13) 0.0268(11) -0.0034(10) -0.0130(10) -0.0045(10) N5 0.0376(13) 0.0260(12) 0.0373(13) 0.0001(10) -0.0192(11) -0.0036(10) C1 0.0317(15) 0.0380(17) 0.0438(16) 0.0002(13) -0.0214(14) -0.0069(12) C2 0.0363(16) 0.0409(17) 0.0378(17) 0.0045(13) -0.0163(15) -0.0062(13) C3 0.0330(15) 0.0367(16) 0.0365(15) -0.0027(12) -0.0174(13) -0.0101(12) C4 0.0300(14) 0.0320(14) 0.0312(14) 0.0013(12) -0.0143(12) -0.0089(11) C5 0.0385(17) 0.058(2) 0.0373(16) -0.0138(15) -0.0171(15) 0.0032(14) C6 0.0395(19) 0.103(3) 0.042(2) -0.025(2) -0.0156(17) 0.003(2) C7 0.0339(19) 0.140(4) 0.0282(17) -0.013(2) -0.0029(16) -0.016(2) C8 0.051(2) 0.092(3) 0.0411(19) 0.0187(19) -0.0213(17) -0.035(2) C9 0.0306(15) 0.0581(19) 0.0287(14) 0.0070(14) -0.0163(13) -0.0170(13) C10 0.0435(17) 0.0404(16) 0.0387(16) 0.0126(13) -0.0277(15) -0.0183(13) C11 0.081(3) 0.053(2) 0.061(2) 0.0222(18) -0.046(2) -0.0367(19) C12 0.111(3) 0.039(2) 0.092(3) 0.021(2) -0.075(3) -0.033(2) C13 0.088(3) 0.0314(18) 0.085(3) -0.0140(18) -0.060(2) 0.0026(17) C14 0.0554(19) 0.0344(17) 0.0538(19) -0.0088(15) -0.0305(17) 0.0014(14) C15 0.0409(18) 0.0451(19) 0.0532(19) -0.0045(15) -0.0305(16) -0.0079(14) C16 0.0365(16) 0.0406(17) 0.0410(17) 0.0033(13) -0.0241(14) -0.0060(13) C17 0.0308(16) 0.0482(18) 0.0477(18) -0.0003(15) -0.0203(15) 0.0002(13) C18 0.049(2) 0.065(2) 0.053(2) -0.0190(18) -0.0245(17) -0.0067(17) C19 0.0356(16) 0.0381(16) 0.0419(17) -0.0005(14) -0.0198(14) -0.0072(13) C20 0.0367(17) 0.063(2) 0.054(2) 0.0025(17) -0.0243(16) 0.0028(15) C21 0.0496(19) 0.064(2) 0.054(2) 0.0121(17) -0.0293(17) -0.0107(16) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 C1 Mo1 C2 81.42(12) C1 Mo1 N2 87.20(9) C2 Mo1 N2 87.59(10) C1 Mo1 C16 103.97(11) C2 Mo1 C16 105.05(11) N2 Mo1 C16 164.09(9) C1 Mo1 N4 101.81(10) C2 Mo1 N4 167.56(10) N2 Mo1 N4 80.62(8) C16 Mo1 N4 85.96(9) C1 Mo1 N5 168.13(9) C2 Mo1 N5 101.35(10) N2 Mo1 N5 81.42(8) C16 Mo1 N5 86.56(9) N4 Mo1 N5 73.11(8) C1 Mo1 C17 108.79(11) C2 Mo1 C17 71.09(11) N2 Mo1 C17 150.42(10) C16 Mo1 C17 35.66(10) N4 Mo1 C17 118.29(10) N5 Mo1 C17 82.94(10) C1 Mo1 C15 70.09(11) C2 Mo1 C15 110.07(12) N2 Mo1 C15 147.94(10) C16 Mo1 C15 35.75(10) N4 Mo1 C15 82.23(10) N5 Mo1 C15 118.85(9) C17 Mo1 C15 61.30(11) C19 O4 C20 115.9(2) N2 N1 C4 105.7(2) N1 N2 N3 113.3(2) N1 N2 Mo1 123.39(16) N3 N2 Mo1 122.84(16) N2 N3 C3 104.5(2) C5 N4 C9 118.5(2) C5 N4 Mo1 123.6(2) C9 N4 Mo1 117.91(18) C14 N5 C10 118.2(2) C14 N5 Mo1 124.60(19) C10 N5 Mo1 117.16(18) O1 C1 Mo1 177.9(2) O2 C2 Mo1 178.1(3) N3 C3 C4 108.9(2) N3 C3 C18 119.0(3) C4 C3 C18 132.1(3) N1 C4 C3 107.6(2) N1 C4 C19 118.9(2) C3 C4 C19 133.5(2) N4 C5 C6 123.4(3) N4 C5 H5 118.3 C6 C5 H5 118.3 C7 C6 C5 118.4(3) C7 C6 H6 120.8 C5 C6 H6 120.8 C6 C7 C8 120.0(3) C6 C7 H7 120.0 C8 C7 H7 120.0 C7 C8 C9 119.6(3) C7 C8 H8 120.2 C9 C8 H8 120.2 N4 C9 C8 120.0(3) N4 C9 C10 115.7(2) C8 C9 C10 124.2(3) N5 C10 C11 121.4(3) N5 C10 C9 116.0(2) C11 C10 C9 122.6(3) C12 C11 C10 119.8(3) C12 C11 H11 120.1 C10 C11 H11 120.1 C13 C12 C11 119.2(3) C13 C12 H12 120.4 C11 C12 H12 120.4 C12 C13 C14 119.3(3) C12 C13 H13 120.4 C14 C13 H13 120.4 N5 C14 C13 121.9(3) N5 C14 H14 119.0 C13 C14 H14 119.0 C16 C15 Mo1 67.53(16) C16 C15 H15A 123.1(18) Mo1 C15 H15A 111.9(18) C16 C15 H15B 116.1(18) Mo1 C15 H15B 110.1(18) H15A C15 H15B 116(3) C17 C16 C15 116.4(3) C17 C16 Mo1 76.70(17) C15 C16 Mo1 76.71(16) C17 C16 H16 121.0(17) C15 C16 H16 122.1(17) Mo1 C16 H16 109.2(17) C16 C17 Mo1 67.63(16) C16 C17 H17A 118.6(18) Mo1 C17 H17A 110.7(17) C16 C17 H17B 121.7(18) Mo1 C17 H17B 111.1(18) H17A C17 H17B 116(3) F1 C18 F2 106.7(3) F1 C18 F3 106.8(3) F2 C18 F3 104.9(3) F1 C18 C3 112.4(3) F2 C18 C3 113.5(3) F3 C18 C3 112.0(3) O3 C19 O4 124.0(3) O3 C19 C4 124.3(3) O4 C19 C4 111.8(2) O4 C20 C21 107.8(2) O4 C20 H20A 110.1 C21 C20 H20A 110.1 O4 C20 H20B 110.1 C21 C20 H20B 110.1 H20A C20 H20B 108.5 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mo1 C1 1.954(3) Mo1 C2 1.964(3) Mo1 N2 2.210(2) Mo1 C16 2.214(3) Mo1 N4 2.218(2) Mo1 N5 2.234(2) Mo1 C17 2.330(3) Mo1 C15 2.332(3) F1 C18 1.312(4) F2 C18 1.314(4) F3 C18 1.327(4) O1 C1 1.156(3) O2 C2 1.150(3) O3 C19 1.197(3) O4 C19 1.333(3) O4 C20 1.455(3) N1 N2 1.328(3) N1 C4 1.343(3) N2 N3 1.340(3) N3 C3 1.342(3) N4 C5 1.351(3) N4 C9 1.351(3) N5 C14 1.346(3) N5 C10 1.351(3) C3 C4 1.387(4) C3 C18 1.482(4) C4 C19 1.480(4) C5 C6 1.361(4) C5 H5 0.9300 C6 C7 1.357(5) C6 H6 0.9300 C7 C8 1.377(5) C7 H7 0.9300 C8 C9 1.395(4) C8 H8 0.9300 C9 C10 1.472(4) C10 C11 1.379(4) C11 C12 1.367(5) C11 H11 0.9300 C12 C13 1.362(5) C12 H12 0.9300 C13 C14 1.385(4) C13 H13 0.9300 C14 H14 0.9300 C15 C16 1.400(4) C15 H15A 0.947(5) C15 H15B 0.950(5) C16 C17 1.396(4) C16 H16 0.950(5) C17 H17A 0.949(5) C17 H17B 0.950(5) C20 C21 1.475(4) C20 H20A 0.9700 C20 H20B 0.9700 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 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 C4 N1 N2 N3 0.1(3) C4 N1 N2 Mo1 -172.04(16) N1 N2 N3 C3 -0.1(3) Mo1 N2 N3 C3 172.13(16) N2 N3 C3 C4 0.0(3) N2 N3 C3 C18 178.9(2) N2 N1 C4 C3 -0.1(3) N2 N1 C4 C19 179.4(2) N3 C3 C4 N1 0.1(3) C18 C3 C4 N1 -178.6(3) N3 C3 C4 C19 -179.3(3) C18 C3 C4 C19 2.1(5) C9 N4 C5 C6 -1.8(4) Mo1 N4 C5 C6 -179.3(2) N4 C5 C6 C7 0.3(5) C5 C6 C7 C8 1.1(5) C6 C7 C8 C9 -0.9(5) C5 N4 C9 C8 2.0(4) Mo1 N4 C9 C8 179.64(19) C5 N4 C9 C10 -175.9(2) Mo1 N4 C9 C10 1.8(3) C7 C8 C9 N4 -0.7(4) C7 C8 C9 C10 177.0(3) C14 N5 C10 C11 -2.8(4) Mo1 N5 C10 C11 178.8(2) C14 N5 C10 C9 175.5(2) Mo1 N5 C10 C9 -2.9(3) N4 C9 C10 N5 0.7(3) C8 C9 C10 N5 -177.0(2) N4 C9 C10 C11 179.1(2) C8 C9 C10 C11 1.3(4) N5 C10 C11 C12 0.7(4) C9 C10 C11 C12 -177.5(3) C10 C11 C12 C13 1.8(5) C11 C12 C13 C14 -2.2(5) C10 N5 C14 C13 2.4(4) Mo1 N5 C14 C13 -179.3(2) C12 C13 C14 N5 0.1(5) Mo1 C15 C16 C17 -67.6(2) C15 C16 C17 Mo1 67.6(2) N3 C3 C18 F1 -11.4(4) C4 C3 C18 F1 167.1(3) N3 C3 C18 F2 -132.7(3) C4 C3 C18 F2 45.9(5) N3 C3 C18 F3 108.8(3) C4 C3 C18 F3 -72.6(4) C20 O4 C19 O3 -2.0(4) C20 O4 C19 C4 177.3(2) N1 C4 C19 O3 18.8(4) C3 C4 C19 O3 -161.9(3) N1 C4 C19 O4 -160.5(2) C3 C4 C19 O4 18.8(4) C19 O4 C20 C21 -179.7(2)