CuI/CuIII prototypical organometallic mechanism for the deactivation of an active pincer-like CuI catalyst in Ullmann-type couplings
Rovira, Mireia; Jašíková, Lucie; Andris, Erik; Acuña-Pares, Ferran; Soler, Marta; Güell, Imma; Wang, Ming-Zheng; Gomez, Laura; Luis, Josep M.; Roithova, Jana; Ribas, Xavi; Chem. Commun.  (2017) –; doi:10.1039/C7CC04491G

data_7120444
_publ_section_title
;
 CuI/CuIII prototypical organometallic mechanism for the deactivation of
 an active pincer-like CuI catalyst in Ullmann-type couplings
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04491G
_journal_year                    2017
_chemical_formula_moiety         'C9 H15 Br Cu N3, 0.33(O H2)'
_chemical_formula_sum            'C9 H15.66 Br Cu N3 O0.33'
_chemical_formula_weight         314.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-17 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.710(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.533(12)
_cell_length_b                   15.50(2)
_cell_length_c                   8.885(11)
_cell_measurement_reflns_used    5681
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.33
_cell_volume                     1202(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13398
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    5.113
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.645998
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             627
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.606
_refine_diff_density_rms
'0.109 &#x00EF;&#x00BB;&#x00BF;#######################################################################'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+1.8506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                2437
_reflns_number_total             2909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc04491g2.cif
_cod_data_source_block           mingbr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7120444