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_1548586
_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         'C25 H17 Au Cl F4 N2 O P'
_chemical_formula_sum            'C25 H17 Au Cl F4 N2 O P'
_chemical_formula_weight         700.79
_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     direct
_audit_creation_date             2015-09-29
_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                90
_cell_angle_beta                 112.700(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.942(2)
_cell_length_b                   10.9697(7)
_cell_length_c                   24.135(2)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      24.3870
_cell_measurement_theta_min      3.7200
_cell_volume                     4870.7(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -170.50 171.50   0.50   30.00   0.00 -10.00  24.00    --   684
  2  \f    132.00 177.00   0.50   30.00   0.00 -10.00 -56.00    --    90
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       '\f scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086761000
_diffrn_orient_matrix_UB_12      0.0050682000
_diffrn_orient_matrix_UB_13      0.0257932000
_diffrn_orient_matrix_UB_21      -0.0303228000
_diffrn_orient_matrix_UB_22      -0.0388597000
_diffrn_orient_matrix_UB_23      -0.0136207000
_diffrn_orient_matrix_UB_31      0.0221952000
_diffrn_orient_matrix_UB_32      -0.0513962000
_diffrn_orient_matrix_UB_33      0.0127958000
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44413
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.333
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.32a (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       needle
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9919
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0668P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6619
_reflns_number_total             9919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy01614j2.cif
_cod_data_source_block           ta1141_mo1
_cod_depositor_comments
'Adding full bibliography for 1548586--1548589.cif.'
_cod_original_cell_volume        4870.6(8)
_cod_database_code               1548586
_chemical_oxdiff_formula         C25H17AuClF4N2OP
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.31
_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. Restrained distances
 N1-C15 = N3-C15 = N2-C19 = N4-C19
 1.42 with sigma of 0.02
 N5-C42 = N7-C42 = N6-C44 = N8-C44
 1.42 with sigma of 0.02
 N7-N8 = N5-N6
 1.24 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N6) = Uanis(N5) = Uanis(N8) = Uanis(N7)
Uanis(N3) = Uanis(N1) = Uanis(N4) = Uanis(N2)
4. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) N4(0.5) N5(0.5) N6(0.5) N7(0.5) N8(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C17(H17), C18(H18), C21(H21), C23(H23), C31(H31), C30(H30), C29(H29),
  C28(H28), C27(H27), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C39(H39), C40(H40), C46(H46), C48(H48)
5.b Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C7(C8,C9,C10,C11,C12), C26(C31,C30,C29,C28,C27), C32(C33,
 C34,C35,C36,C37)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              22559
_shelx_shelxl_version_number     2014/7
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.037
_oxdiff_exptl_absorpt_empirical_full_min 0.668