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_7123157
_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 Fe O2 P'
_chemical_formula_sum            'C14 H17 Fe O2 P'
_chemical_formula_weight         304.09
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-02-19 deposited with the CCDC.    2019-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                82.74(3)
_cell_angle_beta                 89.87(3)
_cell_angle_gamma                82.00(3)
_cell_formula_units_Z            4
_cell_length_a                   9.0780(18)
_cell_length_b                   10.334(2)
_cell_length_c                   14.468(3)
_cell_measurement_reflns_used    26843
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      1.42
_cell_volume                     1333.1(5)
_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    'SIR2004 (Burla et al., 2007)'
_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  0.0852
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21197
_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         27.000
_diffrn_reflns_theta_min         1.419
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.6985
_exptl_absorpt_correction_T_min  0.4415
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       irregular
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0615P)^2^+0.3964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4497
_reflns_number_total             5828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01492f2.cif
_cod_data_source_block           hw_a_CCDC3
_cod_database_code               7123157
_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), C00B(H00B), C10(H10), C00F(H00F), C3(H3), C2(H2), C00J(H00J), C8(H8),
 C9(H9), C5(H5), C00N(H00N), C00O(H00O), C4(H4), C00S(H00S), C00W(H00W),
 C00Y(H00Y)
2.b Idealised Me refined as rotating group:
 C00T(H00A,H00C,H00D), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C00Z(H00E,H00G,H00H), C010(H01A,H01B,H01C)
;
_shelx_res_checksum              49823
_olex2_exptl_crystal_mounting_method 'glass needle'
_olex2_submission_original_sample_id L3
_olex2_submission_special_instructions 'No special instructions were received'