Bimetallic gold(i) complexes of photoswitchable phosphines: synthesis and uses in cooperative catalysis
Arif, T.; Cazorla, C.; Bogliotti, N.; Saleh, N.; Blanchard, F.; Gandon, V.; Métivier, R.; Xie, J.; Voituriez, A.; Marinetti, A.; Catalysis Science & Technology 8 (2018) 710–; doi:10.1039/C7CY01614J

data_1548588
_publ_section_title
;
 Bimetallic gold(i) complexes of photoswitchable phosphines: synthesis and
 uses in cooperative catalysis
;
_journal_issue                   3
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              710
_journal_paper_doi               10.1039/C7CY01614J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety
'2(C18 H12 Au Cl F2 N P), 1.41(C H Cl3), 0.44(C H2 Cl2)'
_chemical_formula_sum            'C37.85 H26.29 Au2 Cl7.11 F4 N2 P2'
_chemical_formula_weight         1293.03
_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             2015-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-10 deposited with the CCDC.
2017-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                109.459(3)
_cell_angle_beta                 103.933(5)
_cell_angle_gamma                104.747(5)
_cell_formula_units_Z            2
_cell_length_a                   11.051(3)
_cell_length_b                   15.816(4)
_cell_length_c                   16.857(5)
_cell_measurement_reflns_used    4916
_cell_measurement_temperature    130
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.6
_cell_volume                     2509.4(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b43 (Rigaku, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b43 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b43 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.0
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -96.0000 - 84.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 14.0000
                 Phi: -144.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 242
               Slice: -96.0000 - 25.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -44.0000
                 Phi: -36.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 167
               Slice: -59.5000 - 24.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -44.0000
                 Phi: -180.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 187
               Slice: -91.5000 - 2.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 144.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 93
               Slice: -30.0000 - 16.5000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -72.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 90
               Slice: -25.0000 - 20.0000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -180.0000
                 XTD: 35.0879
              2theta: -5.9060
scan:
    Number of images: 1
               Slice: 8.0000 - 8.5000
         Image width: 0.5000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 43.0000
                 Phi: 108.0000
                 XTD: 35.0879
              2theta: -5.9060
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.083483
_diffrn_orient_matrix_UB_12      -0.053115
_diffrn_orient_matrix_UB_13      0.015700
_diffrn_orient_matrix_UB_21      -0.041417
_diffrn_orient_matrix_UB_22      0.030326
_diffrn_orient_matrix_UB_23      0.050559
_diffrn_orient_matrix_UB_31      -0.054040
_diffrn_orient_matrix_UB_32      0.032621
_diffrn_orient_matrix_UB_33      -0.023501
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46126
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         3.616
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.325
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224.5
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         5.208
_refine_diff_density_min         -2.737
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9151
_refine_ls_number_restraints     423
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+150.5502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.2689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7354
_reflns_number_total             9151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy01614j2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 1548586--1548589.cif.'
_cod_database_code               1548588
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.364
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9454(12) 0.0546(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, C37, C38, C39, P2, Au2, Cl2, P1, Au1, Cl1, N1, N2, Cl10, Cl9,
 Cl3, Cl5, Cl4, Cl7, Cl8, Cl6, F2, F1, F3, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C37)=Sof(H37)=Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=FVAR(1)
 Sof(C38)=Sof(H38)=Sof(Cl7)=Sof(Cl8)=Sof(Cl6)=FVAR(2)
 Sof(Cl9)=Sof(Cl10)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(3)
5.a Free rotating group:
 Cl9(Cl10,C39)
5.b Ternary CH refined with riding coordinates:
 C37(H37), C38(H38)
5.c Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C17(H17), C18(H18), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              98824
_olex2_submission_special_instructions 'No special instructions were received'