Cooperative C(sp3)‒H and C(sp2)‒H Activation of 2-Ethylpyridines by Copper and Rhodium: A Route toward Quinolizinium Salts
Luo, Ching-Zong; Gandeepan, Parthasarathy; Wu, Yun-Ching; Tsai, Chia-Hung; Cheng, Chien-Hong; ACS Catalysis 5 (2015) 4837–; doi:10.1021/acscatal.5b01244

data_4513443
_publ_section_title
;
 Cooperative C(sp3)--H and C(sp2)--H Activation of 2-Ethylpyridines by
 Copper and Rhodium: A Route toward Quinolizinium Salts
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              4837
_journal_paper_doi               10.1021/acscatal.5b01244
_journal_volume                  5
_journal_year                    2015
_chemical_formula_sum            'C21 H16 F6 N Sb'
_chemical_formula_weight         518.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.371(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.0833(12)
_cell_length_b                   9.1095(8)
_cell_length_c                   33.015(3)
_cell_measurement_reflns_used    7630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3414
_cell_measurement_theta_min      2.7248
_cell_volume                     3933.7(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            15975
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tabullar
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+5.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                3654
_reflns_number_total             3993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5b01244_si_004.cif
_cod_data_source_block           mo_130922lt_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513441--4513443.cif.
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_cod_database_code               4513443