C‒H Activation of Fluoroarenes: Synthesis, Structure, and Luminescence Properties of Copper(I) and Gold(I) Complexes Bearing 2-Phenylpyridine Ligands
Molteni, Roberto; Edkins, Katharina; Haehnel, Martin; Steffen, Andreas; Organometallics 35 (2016) 629–; doi:10.1021/acs.organomet.5b00904

data_4088166
_publ_section_title
;
 C--H Activation of Fluoroarenes: Synthesis, Structure, and Luminescence
 Properties of Copper(I) and Gold(I) Complexes Bearing 2-Phenylpyridine
 Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              629
_journal_paper_doi               10.1021/acs.organomet.5b00904
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C38 H40 Au F4 N3, C H2 Cl2'
_chemical_formula_sum            'C39 H42 Au Cl2 F4 N3'
_chemical_formula_weight         896.62
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.527(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6115(11)
_cell_length_b                   13.9289(12)
_cell_length_c                   21.3841(19)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.19
_cell_volume                     3724.1(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41181
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.819
_diffrn_reflns_theta_min         1.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.146
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0678 before and 0.0462 after correction.
The Ratio of minimum to maximum transmission is 0.8083.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.022
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0261P)^2^+2.0403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6823
_reflns_number_total             7943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00904_si_009.cif
_cod_data_source_block           rmx_0m
_cod_database_code               4088166
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C22(H22), C10(H10), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C35(H35), C20(H20), C8(H8), C6(H6), C3(H3), C36(H36), C37(H37),
 C38(H38), C19(H19), C18(H18), C7(H7)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              73222
_shelx_hkl_checksum              75024
_olex2_submission_special_instructions 'No special instructions were received'