Synthesis of Water-Soluble Gold-Aryl Nanoparticles with Distinct Catalytic Performance in the Reduction of the Environmental Pollutant 4-Nitrophenol
Ahmad, Ahmad A. L.; Panicker, Seema; Chehimi, Mohamed M.; Monge, Miguel; López-de-Luzuriaga, José M.; Mohamed, Ahmed A.; Bruce, Alice E.; Bruce, Mitchell R. M.; Catalysis Science & Technology  (2019) –; doi:10.1039/C9CY01402K

data_1552352
_publ_section_title
;
 Synthesis of Water-Soluble Gold-Aryl Nanoparticles with Distinct
 Catalytic Performance in the Reduction of the Environmental Pollutant
 4-Nitrophenol
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C9CY01402K
_journal_year                    2019
_chemical_formula_moiety         'Au Cl4, C7 H5 N2 O2, H2 O'
_chemical_formula_sum            'C7 H7 Au Cl4 N2 O3'
_chemical_formula_weight         505.91
_chemical_name_systematic        'Gold(III) diazonium salt'
_chemical_properties_physical    Heat-sensitive,Light-sensitive
_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
_audit_creation_date             2019-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-10 deposited with the CCDC.    2019-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                97.173(15)
_cell_angle_beta                 95.533(15)
_cell_angle_gamma                96.097(15)
_cell_formula_units_Z            2
_cell_length_a                   7.831(2)
_cell_length_b                   7.931(2)
_cell_length_c                   11.079(3)
_cell_measurement_reflns_used    2090
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.82
_cell_measurement_theta_min      3.73
_cell_volume                     674.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6474
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.607
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.690
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.2780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1362 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.3730. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.490
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_preparation       'Slow evaporation of acetonitrile solvent.'
_exptl_crystal_recrystallization_method 'Solvent slow evaporation'
_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.127
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.0041(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0317P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1743
_reflns_number_total             2370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy01402k2.cif
_cod_data_source_block           audiz_0m
_cod_original_cell_volume        674.7(3)
_cod_database_code               1552352
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.159
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O3-H7 = O3-H8
 0.9584 with sigma of 0.001
 H7-H8
 1.515 with sigma of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C2(H2), C3(H3)
3.b Fitted hexagon refined as free rotating group:
 C4(C5,C6,C1,C2,C3)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              88135
_olex2_exptl_crystal_mounting_method 'MiTeGen Loop'
_olex2_submission_original_sample_id 'Gold(III) Diazonium salt'
_olex2_submission_special_instructions 'No special instructions were received'