#------------------------------------------------------------------------------ #$Date: 2019-12-24 04:16:54 +0200 (Tue, 24 Dec 2019) $ #$Revision: 245547 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125687.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_7125687 loop_ _publ_author_name 'He, Shichao' 'Allemond, Laynee L.' 'Dunning, Samuel' 'Reynolds III, Joseph' 'Lynch, Vincent' 'Humphrey, Simon M.' _publ_section_title ; In situ formation and solid-state oxidation of a triselenane NSeN-pincer MOF ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC07851G _journal_year 2020 _chemical_formula_moiety 'C6 H5 N O2 Se' _chemical_formula_sum 'C6 H5 N O2 Se' _chemical_formula_weight 202.07 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-09-26 deposited with the CCDC. 2019-12-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.3732(5) _cell_length_b 13.5112(7) _cell_length_c 5.8925(3) _cell_measurement_reflns_used 1983 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 73.1 _cell_measurement_theta_min 6.20 _cell_volume 666.63(6) _computing_cell_refinement 'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction' _computing_data_collection 'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction' _computing_data_reduction 'CrysAlisPro V 1.171.40.53, Rigaku Oxford Diffraction' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material 'Shelxl-2016/6, Sheldrick, G. M.' _computing_structure_refinement 'Shelxl-2016/6, Sheldrick, G. M.' _computing_structure_solution ; SHELXT. Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Agilent SuperNova with an Atlas S2 CCD' _diffrn_measurement_method \w-scans _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 3348 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.070 _diffrn_reflns_theta_min 6.218 _diffrn_source 'microfocus sealed tube' _exptl_absorpt_coefficient_mu 7.095 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.396 _exptl_absorpt_correction_type 'gaussian and multi-scan' _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.013 _exptl_crystal_description needle _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.590 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.651 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.100 _refine_ls_abs_structure_details ; Flack x determined using 524 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 1287 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0325 _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^)+(0.0669P)^2^+0.5547P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.0880 _reflns_Friedel_coverage 0.753 _reflns_Friedel_fraction_full 0.951 _reflns_Friedel_fraction_max 0.904 _reflns_number_gt 1268 _reflns_number_total 1287 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc07851g2.cif _cod_data_source_block sh17035 _cod_database_code 7125687 _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. ; _shelx_estimated_absorpt_t_min 0.102 _shelx_estimated_absorpt_t_max 0.815 _shelx_res_file ; TITL shelxt_b.res in Pna2(1) yellow needle shelx.res created by SHELXL-2016/6 at 13:13:26 on 25-Jul-2019 CELL 1.54184 8.3732 13.5112 5.8925 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0007 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O SE UNIT 24 20 4 8 4 MERG 2 FMAP 2 SIZE 0.030 0.035 0.590 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -173.00 WGHT 0.066900 0.554700 FVAR 6.24126 SE1 5 0.672908 0.095641 0.311889 11.00000 0.02440 0.01839 = 0.02737 0.00119 0.00379 0.00109 N1 3 0.757235 0.284073 0.179199 11.00000 0.02300 0.02298 = 0.01981 -0.00130 -0.00003 0.00226 AFIX 43 H1N 2 0.809254 0.249407 0.076627 11.00000 -1.20000 AFIX 0 O1 4 0.471758 0.154068 0.709482 11.00000 0.03481 0.02465 = 0.03014 0.00120 0.00791 -0.00529 AFIX 147 H1A 2 0.524352 0.125163 0.607779 11.00000 -1.50000 AFIX 0 O2 4 0.432360 0.305908 0.834181 11.00000 0.03303 0.03007 = 0.02718 0.00170 0.01068 0.00074 C2 1 0.671084 0.233387 0.336121 11.00000 0.01410 0.02185 = 0.02847 0.00450 -0.00557 -0.00164 C3 1 0.592049 0.291023 0.502156 11.00000 0.01264 0.02125 = 0.02220 0.00253 -0.00190 0.00238 C4 1 0.602149 0.393613 0.490922 11.00000 0.01665 0.02669 = 0.01960 -0.00049 -0.00125 0.00214 AFIX 43 H4 2 0.546524 0.432103 0.600265 11.00000 -1.20000 AFIX 0 C5 1 0.689970 0.441161 0.326809 11.00000 0.01974 0.02128 = 0.02441 -0.00329 0.00677 -0.00345 AFIX 43 H5 2 0.696235 0.511334 0.321932 11.00000 -1.20000 AFIX 0 C6 1 0.769065 0.383191 0.168693 11.00000 0.02581 0.02174 = 0.01894 0.00021 0.00320 0.00005 AFIX 43 H6 2 0.831459 0.413401 0.053223 11.00000 -1.20000 AFIX 0 C7 1 0.494813 0.250564 0.694116 11.00000 0.02015 0.02324 = 0.02509 0.00110 0.00265 0.00150 HKLF 4 REM shelxt_b.res in Pna2(1) yellow needle REM R1 = 0.0325 for 1268 Fo > 4sig(Fo) and 0.0329 for all 1287 data REM 92 parameters refined using 1 restraints END WGHT 0.0602 0.3226 REM Highest difference peak 0.651, deepest hole -0.508, 1-sigma level 0.100 Q1 1 0.8310 0.0971 0.3139 11.00000 0.05 0.65 Q2 1 0.5041 0.0945 0.3132 11.00000 0.05 0.63 Q3 1 0.6380 0.0979 0.4525 11.00000 0.05 0.60 Q4 1 0.6308 0.0951 0.1741 11.00000 0.05 0.59 Q5 1 0.7107 0.0936 0.4516 11.00000 0.05 0.58 Q6 1 0.7129 0.0945 0.1822 11.00000 0.05 0.54 Q7 1 0.4236 0.1971 0.8171 11.00000 0.05 0.41 Q8 1 0.6759 0.4266 0.2098 11.00000 0.05 0.33 Q9 1 0.6681 0.1980 0.3259 11.00000 0.05 0.29 Q10 1 0.9112 0.2594 0.3342 11.00000 0.05 0.29 Q11 1 0.3851 0.3444 0.9661 11.00000 0.05 0.28 Q12 1 0.6576 0.2398 0.4830 11.00000 0.05 0.27 Q13 1 0.6698 -0.0376 0.1777 11.00000 0.05 0.27 Q14 1 0.6548 0.4116 0.3971 11.00000 0.05 0.27 Q15 1 0.7116 0.1816 0.3469 11.00000 0.05 0.27 Q16 1 0.9956 0.3797 0.1405 11.00000 0.05 0.26 Q17 1 0.6043 0.1732 0.8041 11.00000 0.05 0.26 Q18 1 0.7417 0.2616 0.3053 11.00000 0.05 0.25 Q19 1 0.9974 0.4162 0.0874 11.00000 0.05 0.25 Q20 1 0.5077 0.2681 0.8155 11.00000 0.05 0.25 ; _shelx_res_checksum 6939 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, 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 Se1 Se 0.67291(6) 0.09564(3) 0.3119(2) 0.0234(2) Uani 1 1 d . . N1 N 0.7572(6) 0.2841(3) 0.1792(8) 0.0219(9) Uani 1 1 d . . H1N H 0.809254 0.249407 0.076627 0.026 Uiso 1 1 calc R U O1 O 0.4718(6) 0.1541(3) 0.7095(7) 0.0299(9) Uani 1 1 d . . H1A H 0.524352 0.125163 0.607779 0.045 Uiso 1 1 calc R U O2 O 0.4324(5) 0.3059(3) 0.8342(9) 0.0301(9) Uani 1 1 d . . C2 C 0.6711(5) 0.2334(4) 0.3361(17) 0.0215(14) Uani 1 1 d . . C3 C 0.5920(6) 0.2910(4) 0.5022(9) 0.0187(10) Uani 1 1 d . . C4 C 0.6021(7) 0.3936(4) 0.4909(10) 0.0210(11) Uani 1 1 d . . H4 H 0.546524 0.432103 0.600265 0.025 Uiso 1 1 calc R U C5 C 0.6900(5) 0.4412(4) 0.3268(18) 0.0218(11) Uani 1 1 d . . H5 H 0.696235 0.511334 0.321932 0.026 Uiso 1 1 calc R U C6 C 0.7691(7) 0.3832(4) 0.1687(9) 0.0222(10) Uani 1 1 d . . H6 H 0.831459 0.413401 0.053223 0.027 Uiso 1 1 calc R U C7 C 0.4948(7) 0.2506(4) 0.6941(9) 0.0228(11) Uani 1 1 d . . 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 Se1 0.0244(4) 0.0184(3) 0.0274(3) 0.0012(3) 0.0038(4) 0.00109(16) N1 0.023(2) 0.023(2) 0.020(2) -0.0013(16) 0.0000(19) 0.0023(18) O1 0.035(2) 0.0246(19) 0.0301(19) 0.0012(16) 0.0079(18) -0.0053(17) O2 0.033(2) 0.0301(17) 0.027(2) 0.002(2) 0.011(2) 0.0007(15) C2 0.014(2) 0.022(2) 0.028(4) 0.005(3) -0.006(3) -0.0016(16) C3 0.013(2) 0.021(2) 0.022(2) 0.0025(19) -0.002(2) 0.0024(19) C4 0.017(3) 0.027(3) 0.020(2) -0.0005(19) -0.001(2) 0.002(2) C5 0.020(2) 0.021(2) 0.024(3) -0.003(3) 0.007(3) -0.0034(17) C6 0.026(3) 0.022(2) 0.019(2) 0.000(2) 0.003(2) 0.000(2) C7 0.020(3) 0.023(2) 0.025(3) 0.001(2) 0.003(2) 0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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 C6 N1 C2 124.9(5) C6 N1 H1N 117.5 C2 N1 H1N 117.5 C7 O1 H1A 109.5 N1 C2 C3 116.2(5) N1 C2 Se1 116.5(5) C3 C2 Se1 127.3(5) C4 C3 C2 119.2(5) C4 C3 C7 115.7(5) C2 C3 C7 125.2(5) C5 C4 C3 122.1(5) C5 C4 H4 118.9 C3 C4 H4 118.9 C4 C5 C6 117.7(5) C4 C5 H5 121.2 C6 C5 H5 121.2 N1 C6 C5 119.8(5) N1 C6 H6 120.1 C5 C6 H6 120.1 O2 C7 O1 119.5(5) O2 C7 C3 121.1(5) O1 C7 C3 119.4(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 C2 1.867(5) N1 C6 1.344(8) N1 C2 1.358(9) N1 H1N 0.8800 O1 C7 1.321(7) O1 H1A 0.8400 O2 C7 1.230(7) C2 C3 1.415(9) C3 C4 1.390(7) C3 C7 1.497(7) C4 C5 1.374(10) C4 H4 0.9500 C5 C6 1.386(10) C5 H5 0.9500 C6 H6 0.9500 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 C6 N1 C2 C3 -1.5(9) C6 N1 C2 Se1 179.5(4) N1 C2 C3 C4 2.2(8) Se1 C2 C3 C4 -179.0(5) N1 C2 C3 C7 -178.2(5) Se1 C2 C3 C7 0.7(9) C2 C3 C4 C5 -1.7(9) C7 C3 C4 C5 178.6(6) C3 C4 C5 C6 0.4(9) C2 N1 C6 C5 0.3(9) C4 C5 C6 N1 0.4(9) C4 C3 C7 O2 -1.8(8) C2 C3 C7 O2 178.6(6) C4 C3 C7 O1 176.2(5) C2 C3 C7 O1 -3.5(9)