Simple synthetic access to [Au(IBiox)Cl] complexes
Martynova, Ekaterina A.; Zuccarello, Marco; kronenberg, domenic; Belis, Marek; Cavallo, Luigi; Baudoin, Olivier; Kwit, Marcin; Van Hecke, Kristof; Zhang, Ziyun; czapik, agnieszka; Nolan, Steven P.; Dalton Transactions  (2023) –; doi:10.1039/D3DT01357J

data_7713004
_publ_section_title
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 Simple synthetic access to [Au(IBiox)Cl] complexes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01357J
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H20 Au Cl N2 O2'
_chemical_formula_sum            'C13 H20 Au Cl N2 O2'
_chemical_formula_weight         468.73
_chemical_name_systematic        Au(IBiox-iPr)Cl
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-05
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2023-01-26 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.23112(15)
_cell_length_b                   11.8487(3)
_cell_length_c                   18.5359(4)
_cell_measurement_reflns_used    11026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.9000
_cell_measurement_theta_min      2.7750
_cell_volume                     1588.14(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -64.00  35.00   1.00   10.00    --   10.17 -38.00 120.00   99
  2  \w    -15.00  51.00   1.00   10.00    --   10.17 -99.00 -90.00   66
  3  \w    -64.00  35.00   1.00   10.00    --   10.17 -38.00 -60.00   99
  4  \w    -18.00  83.00   1.00   10.00    --   10.17  57.00  90.00  101
  5  \w    -18.00  83.00   1.00   10.00    --   10.17  57.00 -90.00  101
  6  \w     37.00  97.00   1.00   10.00    --   10.17-178.00 150.00   60
  7  \w    -42.00  21.00   1.00   10.00    --  -11.11 -77.00  90.00   63
  8  \w    -44.00  21.00   1.00   10.00    --  -11.11  77.00   0.00   65
  9  \w    -44.00  21.00   1.00   10.00    --  -11.11  77.00 120.00   65
 10  \w    -44.00 -19.00   1.00   10.00    --  -11.11  77.00-120.00   25
 11  \w    -15.00  30.00   1.00   10.00    --  -11.11 -99.00 -90.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0096255000
_diffrn_orient_matrix_UB_12      0.0590317000
_diffrn_orient_matrix_UB_13      0.0051161000
_diffrn_orient_matrix_UB_21      -0.0773598000
_diffrn_orient_matrix_UB_22      0.0095364000
_diffrn_orient_matrix_UB_23      -0.0227307000
_diffrn_orient_matrix_UB_31      -0.0595367000
_diffrn_orient_matrix_UB_32      -0.0028220000
_diffrn_orient_matrix_UB_33      0.0303545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.692
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.431
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_preparation       Synthesis
_exptl_crystal_recrystallization_method 'Hexane diffusion in CHCl3'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0143P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2773
_reflns_number_total             4248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01357j2.cif
_cod_data_source_block           em-au(ibiox-ipr)cl
_cod_database_code               7713004
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C13 H20 Au Cl N2 O2'
_shelx_estimated_absorpt_t_max   0.584
_shelx_estimated_absorpt_t_min   0.374
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              48828
_olex2_date_sample_data_collection 2022-08-04
_olex2_exptl_crystal_mounting_method 'Litho loop'
_olex2_submission_original_sample_id Au(IBiox-iPr)Cl
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.823