#------------------------------------------------------------------------------ #$Date: 2021-09-06 14:48:17 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268827 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/30/7243091.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_7243091 loop_ _publ_author_name 'Kusy, Rafa\/l' 'Grela, Karol' _publ_section_title ; Ligand-free (Z)-selective transfer semihydrogenation of alkynes catalyzed by in situ generated oxidizable copper nanoparticles ; _journal_issue 15 _journal_name_full 'Green Chemistry' _journal_page_first 5494 _journal_page_last 5502 _journal_paper_doi 10.1039/D1GC01206A _journal_volume 23 _journal_year 2021 _chemical_formula_moiety 'N H4 [B5 O10 H4], 2(H2 O)' _chemical_formula_sum 'B5 H12 N O12' _chemical_formula_weight 272.16 _chemical_name_systematic 'Ammonium pentaborate' _space_group_crystal_system orthorhombic _space_group_IT_number 41 _space_group_name_Hall 'A 2 -2ab' _space_group_name_H-M_alt 'A e a 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2013 _audit_update_record ; 2021-06-09 deposited with the CCDC. 2021-06-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.3246(3) _cell_length_b 11.0147(3) _cell_length_c 9.1513(3) _cell_measurement_reflns_used 1531 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 29.4580 _cell_measurement_theta_min 3.3940 _cell_volume 1141.51(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100.0(1) _diffrn_detector_area_resol_mean 16.2974 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.904 _diffrn_measurement_device_type 'SuperNova (Mo) X-ray Source' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.904 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2278 _diffrn_reflns_point_group_measured_fraction_full 0.892 _diffrn_reflns_point_group_measured_fraction_max 0.762 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.096 _diffrn_reflns_theta_min 3.408 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.584 _exptl_crystal_description prism _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.181 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details ; Flack x determined using 442 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.2(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 97 _refine_ls_number_reflns 1271 _refine_ls_number_restraints 5 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0297 _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^)+(0.0411P)^2^+0.1907P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.0764 _reflns_Friedel_coverage 0.593 _reflns_Friedel_fraction_full 0.769 _reflns_Friedel_fraction_max 0.603 _reflns_number_gt 1217 _reflns_number_total 1271 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1gc01206a1.cif _cod_data_source_block grela_1 _cod_depositor_comments 'Adding full bibliography for 7243091.cif.' _cod_original_sg_symbol_Hall 'A 2 -2ac' _cod_original_sg_symbol_H-M 'A b a 2' _cod_original_formula_sum 'H12 B5 N O12' _cod_database_code 7243091 _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 0.962 _shelx_estimated_absorpt_t_max 0.981 _shelxl_version_number 2013-3 _shelx_res_file ; TITL GRELA_1 in Aea2 CELL 0.71073 11.3246 11.0147 9.1513 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0003 0.000 0.000 0.000 LATT -5 SYMM - X, - Y, Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, Z SFAC B N O H UNIT 20 4 48 48 MERG 2 OMIT -3.00 180.00 dfix 0.85 o1w h1w1 o1w h2w1 n1 h1n1 n1 h2n1 FMAP 2 PLAN 20 ACTA BOND L.S. 20 TEMP -173.00 size 0.25 0.17 0.12 WGHT 0.041100 0.190700 FVAR 5.22661 mole 1 O1W 3 0.972535 0.823325 0.451555 11.00000 0.01450 0.01449 = 0.01848 -0.00221 -0.00366 0.00279 H1W1 4 0.997937 0.752040 0.433991 11.00000 -1.50000 H2W1 4 1.003624 0.845532 0.529684 11.00000 -1.50000 mole 2 N1 2 0.000000 1.000000 0.208887 10.50000 0.01074 0.02070 = 0.01520 0.00000 0.00000 -0.00012 H1N1 4 0.027900 1.053470 0.265272 11.00000 -1.50000 H2N1 4 -0.056655 1.029844 0.158858 11.00000 -1.50000 mole 3 B2 1 0.500000 1.000000 0.292884 10.50000 0.00884 0.01336 = 0.01277 0.00000 0.00000 0.00091 O4 3 0.417936 0.931947 0.198216 11.00000 0.00932 0.01579 = 0.01405 -0.00403 0.00006 0.00071 O3 3 0.563330 0.912684 0.387195 11.00000 0.01053 0.01357 = 0.01546 0.00373 0.00007 0.00058 O2 3 0.736565 0.821234 0.478038 11.00000 0.01158 0.01917 = 0.02525 0.01078 -0.00076 -0.00018 AFIX 147 H2 4 0.810033 0.825095 0.466287 11.00000 -1.50000 AFIX 0 O1 3 0.753136 0.970191 0.295797 11.00000 0.00981 0.01739 = 0.02065 0.00904 0.00098 0.00076 O5 3 0.222573 0.888261 0.112913 11.00000 0.01196 0.02773 = 0.03070 -0.01857 -0.00347 0.00309 AFIX 147 H5 4 0.258563 0.833267 0.067520 11.00000 -1.50000 AFIX 0 B1 1 0.682656 0.901966 0.387427 11.00000 0.01327 0.01181 = 0.01418 0.00125 -0.00079 -0.00131 B3 1 0.299347 0.947893 0.201499 11.00000 0.01315 0.01496 = 0.01579 -0.00234 -0.00021 0.00028 HKLF 4 REM GRELA_1 in Aea2 REM R1 = 0.0297 for 1217 Fo > 4sig(Fo) and 0.0314 for all 1271 data REM 97 parameters refined using 5 restraints END WGHT 0.0384 0.1919 REM Highest difference peak 0.181, deepest hole -0.222, 1-sigma level 0.052 Q1 1 0.8284 0.8134 0.2197 11.00000 0.05 0.18 Q2 1 0.0644 1.1310 0.1182 11.00000 0.05 0.17 Q3 1 0.8656 0.8512 0.6191 11.00000 0.05 0.17 Q4 1 0.6236 0.8137 0.1990 11.00000 0.05 0.17 Q5 1 0.3628 0.9648 0.1659 11.00000 0.05 0.16 Q6 1 1.0940 0.8056 0.3070 11.00000 0.05 0.16 Q7 1 0.9041 0.8222 0.4220 11.00000 0.05 0.16 Q8 1 0.2092 0.8293 0.1839 11.00000 0.05 0.15 Q9 1 0.0864 1.1888 0.2241 11.00000 0.05 0.14 Q10 1 0.4307 0.8517 0.2225 11.00000 0.05 0.14 Q11 1 0.1299 0.8451 -0.0476 11.00000 0.05 0.14 Q12 1 0.3608 0.9133 0.2427 11.00000 0.05 0.14 Q13 1 1.0912 0.6706 0.5407 11.00000 0.05 0.13 Q14 1 0.8443 0.6694 0.3663 11.00000 0.05 0.13 Q15 1 0.5626 0.8449 0.2724 11.00000 0.05 0.13 Q16 1 0.9567 0.7178 0.2971 11.00000 0.05 0.13 Q17 1 0.2763 0.7622 0.2170 11.00000 0.05 0.13 Q18 1 0.1613 0.8310 0.3161 11.00000 0.05 0.13 Q19 1 0.0195 1.2166 0.2004 11.00000 0.05 0.13 Q20 1 0.6095 0.8643 0.3480 11.00000 0.05 0.12 ; _shelx_res_checksum 42198 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, 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 O1W O 0.97253(12) 0.82333(13) 0.45156(18) 0.0158(3) Uani 1 1 d D . . . . H1W1 H 0.998(2) 0.752(2) 0.434(3) 0.024 Uiso 1 1 d D U . . . H2W1 H 1.004(2) 0.846(3) 0.530(3) 0.024 Uiso 1 1 d D U . . . N1 N 0.0000 1.0000 0.2089(3) 0.0155(5) Uani 1 2 d DS T P . . H1N1 H 0.028(2) 1.053(2) 0.265(3) 0.023 Uiso 1 1 d D U . . . H2N1 H -0.057(2) 1.030(2) 0.159(3) 0.023 Uiso 1 1 d D U . . . B2 B 0.5000 1.0000 0.2929(4) 0.0117(6) Uani 1 2 d S T P . . O4 O 0.41794(12) 0.93195(12) 0.19822(16) 0.0131(3) Uani 1 1 d . . . . . O3 O 0.56333(12) 0.91268(12) 0.38719(17) 0.0132(3) Uani 1 1 d . . . . . O2 O 0.73656(12) 0.82123(13) 0.47804(18) 0.0187(4) Uani 1 1 d . . . . . H2 H 0.8100 0.8251 0.4663 0.028 Uiso 1 1 calc R U . . . O1 O 0.75314(14) 0.97019(13) 0.29580(18) 0.0159(3) Uani 1 1 d . . . . . O5 O 0.22257(13) 0.88826(15) 0.11291(19) 0.0235(4) Uani 1 1 d . . . . . H5 H 0.2586 0.8333 0.0675 0.035 Uiso 1 1 calc R U . . . B1 B 0.68266(19) 0.90197(19) 0.3874(3) 0.0131(4) Uani 1 1 d . . . . . B3 B 0.2993(2) 0.94789(19) 0.2015(3) 0.0146(4) 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 O1W 0.0145(7) 0.0145(6) 0.0185(7) -0.0022(6) -0.0037(6) 0.0028(6) N1 0.0107(12) 0.0207(12) 0.0152(12) 0.000 0.000 -0.0001(10) B2 0.0088(13) 0.0134(13) 0.0128(13) 0.000 0.000 0.0009(11) O4 0.0093(7) 0.0158(6) 0.0140(7) -0.0040(6) 0.0001(6) 0.0007(5) O3 0.0105(6) 0.0136(6) 0.0155(7) 0.0037(5) 0.0001(6) 0.0006(5) O2 0.0116(6) 0.0192(7) 0.0253(9) 0.0108(6) -0.0008(6) -0.0002(6) O1 0.0098(6) 0.0174(6) 0.0206(7) 0.0090(6) 0.0010(6) 0.0008(5) O5 0.0120(8) 0.0277(8) 0.0307(10) -0.0186(7) -0.0035(6) 0.0031(6) B1 0.0133(10) 0.0118(9) 0.0142(10) 0.0012(8) -0.0008(10) -0.0013(8) B3 0.0132(10) 0.0150(10) 0.0158(10) -0.0023(9) -0.0002(9) 0.0003(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source B B 0.0013 0.0007 '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' H H 0.0000 0.0000 '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 O4 B2 O4 108.1(2) 2_675 . ? O4 B2 O3 111.59(7) 2_675 . ? O4 B2 O3 108.54(8) . . ? O4 B2 O3 108.54(8) 2_675 2_675 ? O4 B2 O3 111.59(7) . 2_675 ? O3 B2 O3 108.5(2) . 2_675 ? B3 O4 B2 123.07(15) . . ? B1 O3 B2 122.75(15) . . ? B1 O1 B3 119.07(17) . 2_675 ? O3 B1 O2 120.32(18) . . ? O3 B1 O1 121.85(19) . . ? O2 B1 O1 117.82(18) . . ? O4 B3 O5 123.96(19) . . ? O4 B3 O1 121.64(19) . 2_675 ? O5 B3 O1 114.39(18) . 2_675 ? 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 B2 O4 1.475(2) 2_675 ? B2 O4 1.475(2) . ? B2 O3 1.478(2) . ? B2 O3 1.478(2) 2_675 ? O4 B3 1.355(3) . ? O3 B1 1.356(3) . ? O2 B1 1.361(3) . ? O1 B1 1.380(3) . ? O1 B3 1.383(3) 2_675 ? O5 B3 1.358(3) . ? B3 O1 1.383(3) 2_675 ?