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_4088171
_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         'C42 H31 Br F4 P2 Pd'
_chemical_formula_sum            'C42 H31 Br F4 P2 Pd'
_chemical_formula_weight         859.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-02-08
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.1090(3)
_cell_length_b                   23.1668(6)
_cell_length_c                   25.8891(7)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.36
_cell_volume                     7262.6(3)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            117296
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0777 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.6572.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5729
_exptl_crystal_description       plate
_exptl_crystal_F_000             3433.0105
_exptl_crystal_preparation       'soaked in perfluoro polyether oil'
_exptl_crystal_recrystallization_method 'from toluene'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5411
_refine_diff_density_min         -1.9273
_refine_diff_density_rms         0.1573
_refine_ls_d_res_high            0.8106
_refine_ls_d_res_low             12.9445
_refine_ls_goodness_of_fit_ref   1.0230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    65
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0230
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+5.9331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                5335
_reflns_number_total             7128
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            om5b00904_si_007.cif
_cod_data_source_block           13S010
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088171
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H53 of C53, H51 of C51, H50 of C50, H49 of C49, H48 of C48, H47 of C47, H45
  of C45, H44 of C44, H43 of C43, H8 of C8, H18 of C18, H15 of C15, H14 of C14,
  H12 of C12, H20 of C20, H21 of C21, H22 of C22, H25 of C25, H27 of C27, H28
  of C28, H30 of C30, H31 of C31, H32 of C32, H33 of C33, H34 of C34, H36 of
  C36, H37 of C37, H38 of C38, H39 of C39, H40 of C40, H41 of C41, H42 of C42
2. Others
 Sof(H44)=1-Sof(H51)=1-Sof(H51)=Sof(F2)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C14(H14), C15(H15), C18(H18), C20(H20), C21(H21), C22(H22),
 C25(H25), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53)
;