#------------------------------------------------------------------------------ #$Date: 2019-11-28 19:31:41 +0200 (Thu, 28 Nov 2019) $ #$Revision: 244411 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/63/1556381.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_1556381 loop_ _publ_author_name 'de Almeida, M. Peixoto' 'Martins, L. M. D. R. S.' 'Carabineiro, S. A. C.' 'Lauterbach, T.' 'Rominger, F.' 'Hashmi, A. S. K.' 'Pombeiro, A. J. L.' 'Figueiredo, J. L.' _publ_section_title ; Homogeneous and heterogenised new gold C-scorpionate complexes as catalysts for cyclohexane oxidation ; _journal_issue 11 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 3056 _journal_paper_doi 10.1039/c3cy00552f _journal_volume 3 _journal_year 2013 _chemical_formula_sum 'C3 H5 Au Cl4 N2' _chemical_formula_weight 407.86 _space_group_IT_number 10 _space_group_name_Hall '-P 2y' _space_group_name_H-M_alt 'P 1 2/m 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 98.573(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 3.8864(5) _cell_length_b 7.7824(9) _cell_length_c 7.5103(9) _cell_measurement_reflns_used 2067 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 25.04 _cell_measurement_theta_min 2.62 _cell_volume 224.61(5) _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-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II Quazar' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'ImuS microsource' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2048 _diffrn_reflns_theta_full 25.04 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 2.62 _exptl_absorpt_coefficient_mu 17.492 _exptl_absorpt_correction_T_max 0.4200 _exptl_absorpt_correction_T_min 0.1550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 184 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.791 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.142 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 433 _refine_ls_number_restraints 23 _refine_ls_restrained_S_all 1.168 _refine_ls_R_factor_all 0.0130 _refine_ls_R_factor_gt 0.0130 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0317 _reflns_number_gt 433 _reflns_number_total 433 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c3cy00552f.txt _cod_data_source_block tla21 _cod_depositor_comments ; The following automatic conversions were performed: data item '_symmetry_cell_setting' value 'Monoclinic' was changed to 'monoclinic' in accordance with the /home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/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 6909 2019-04-08 15:41:33Z antanas ; _cod_original_sg_symbol_H-M P2/m _cod_database_code 1556381 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' '-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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.5000 0.5000 0.0000 0.01979(11) Uani 1 4 d SU . . Cl1 Cl 0.5000 0.20685(15) 0.0000 0.0339(3) Uani 1 2 d SU . . Cl2 Cl 0.6568(4) 0.5000 -0.28035(17) 0.0348(3) Uani 1 2 d SU . . C1 C 0.982(3) 0.018(3) -0.3883(16) 0.040(3) Uiso 0.15 1 d PDU A -1 H1 H 0.8932 0.0327 -0.2782 0.048 Uiso 0.25 1 calc PR A -1 C2 C 1.054(5) 0.1432(15) -0.503(3) 0.019(4) Uiso 0.15 1 d PDU A -1 H2 H 1.0435 0.2630 -0.4803 0.023 Uiso 0.25 1 calc PR A -1 C3 C 1.143(5) 0.073(2) -0.655(2) 0.024(4) Uiso 0.15 1 d PDU A -1 H3 H 1.1809 0.1332 -0.7609 0.029 Uiso 0.25 1 calc PR A -1 C4 C 1.166(5) -0.099(2) -0.627(2) 0.032(5) Uiso 0.15 1 d PDU A -1 H4 H 1.2402 -0.1814 -0.7069 0.038 Uiso 0.25 1 calc PR A -1 C5 C 1.065(10) -0.133(2) -0.464(3) 0.057(8) Uiso 0.15 1 d PDU A -1 H5 H 1.0546 -0.2437 -0.4121 0.068 Uiso 0.25 1 calc PR A -1 N1 N 0.982(3) 0.018(3) -0.3883(16) 0.040(3) Uiso 0.10 1 d PU B -2 N2 N 1.054(5) 0.1432(15) -0.503(3) 0.019(4) Uiso 0.10 1 d PU B -2 N3 N 1.143(5) 0.073(2) -0.655(2) 0.024(4) Uiso 0.10 1 d PU B -2 N4 N 1.166(5) -0.099(2) -0.627(2) 0.032(5) Uiso 0.10 1 d PU B -2 N5 N 1.065(10) -0.133(2) -0.464(3) 0.057(8) Uiso 0.10 1 d PU B -2 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 Au1 0.02486(14) 0.01694(15) 0.01796(15) 0.000 0.00445(9) 0.000 Cl1 0.0524(7) 0.0174(6) 0.0342(6) 0.000 0.0141(5) 0.000 Cl2 0.0528(7) 0.0311(6) 0.0238(6) 0.000 0.0163(5) 0.000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 Cl2 Au1 Cl2 180.0 3_665 . Cl2 Au1 Cl1 90.0 3_665 3_665 Cl2 Au1 Cl1 90.0 . 3_665 Cl2 Au1 Cl1 90.0 3_665 . Cl2 Au1 Cl1 90.0 . . Cl1 Au1 Cl1 180.0 3_665 . C2 C1 C5 105.5(9) . . C3 C2 C1 110.5(10) . . C2 C3 C4 106.6(12) . . C3 C4 C5 108.0(12) . . C4 C5 C1 108.9(11) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Au1 Cl2 2.2776(12) 3_665 Au1 Cl2 2.2776(12) . Au1 Cl1 2.2814(12) 3_665 Au1 Cl1 2.2814(12) . C1 C2 1.357(12) . C1 C5 1.367(14) . C2 C3 1.355(13) . C3 C4 1.359(14) . C4 C5 1.365(15) .