Redox-Responsive Phosphonite Gold Complexes in Hydroamination Catalysis
Deck, Eva; Wagner, Hanna E.; Paradies, Jan; Breher, Frank; Chemical Communications  (2019) –; doi:10.1039/C9CC01492F

data_7123155
_publ_section_title
;
 Redox-Responsive Phosphonite Gold Complexes in Hydroamination Catalysis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01492F
_journal_year                    2019
_chemical_formula_moiety         'C34 H33 Au Cl Fe O2 P'
_chemical_formula_sum            'C34 H33 Au Cl Fe O2 P'
_chemical_formula_weight         792.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-19 deposited with the CCDC.    2019-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.49(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0090(16)
_cell_length_b                   25.366(5)
_cell_length_c                   14.803(3)
_cell_measurement_reflns_used    34700
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.73
_cell_measurement_theta_min      1.41
_cell_volume                     2936.2(11)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.622
_exptl_absorpt_coefficient_mu    5.661
_exptl_absorpt_correction_T_max  0.7598
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.055
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00375(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+2.5857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5996
_reflns_number_total             6745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01492f2.cif
_cod_data_source_block           hw_a_CCDC2
_cod_database_code               7123155
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C5(H5), C110(H110), C108(H108), C104(H104), C3(H3),
 C117(H117), C2(H2), C119(H119), C4(H4), C9(H9), C103(H103), C102(H102)
2.b Idealised Me refined as rotating group:
 C114(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C123(H12D,H12E,H12F), C122(H12G,H12H,H12I)
;
_shelx_res_checksum              96235
_olex2_exptl_crystal_mounting_method 'glass needle'
_olex2_submission_original_sample_id ED160
_olex2_submission_special_instructions 'No special instructions were received'