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_7123154
_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         'C14 H17 Au Cl Fe O2 P'
_chemical_formula_sum            'C14 H17 Au Cl Fe O2 P'
_chemical_formula_weight         536.51
_chemical_name_systematic        ED202
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.65(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.374(3)
_cell_length_b                   12.972(3)
_cell_length_c                   18.223(4)
_cell_measurement_reflns_used    45868
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.79
_cell_measurement_theta_min      1.53
_cell_volume                     3160.2(12)
_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 1.000
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49558
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.863
_exptl_absorpt_coefficient_mu    10.459
_exptl_absorpt_correction_T_max  0.7320
_exptl_absorpt_correction_T_min  0.1065
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00089(6)
_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   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+4.7969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5943
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01492f2.cif
_cod_data_source_block           hw_a_CCDC1
_cod_original_cell_volume        3160.2(11)
_cod_database_code               7123154
_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:
 C103(H103), C7(H7), C109(H109), C5(H5), C104(H104), C102(H102), C101(H101),
 C8(H8), C2(H2), C106(H106), C107(H107), C10(H10), C3(H3), C108(H108), C9(H9),
 C4(H4)
2.b Idealised Me refined as rotating group:
 C113(H11A,H11B,H11C), C111(H11D,H11E,H11F), C13(H13A,H13B,H13C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C112(H11G,H11H,H11I)
;
_shelx_res_checksum              96013
_olex2_exptl_crystal_mounting_method 'glass needle'
_olex2_submission_special_instructions 'No special instructions were received'