About the selectivity and reactivity of active nickel electrodes in C‒C coupling reactions
Beil, Sebastian B.; Breiner, Manuel; Schulz, Lara; Schüll, Aaron; Müller, Timo; Schollmeyer, Dieter; Bomm, Alexander; Holtkamp, Michael; Karst, Uwe; Schade, Wolfgang; Waldvogel, Siegfried R.; RSC Advances 10 (2020) 14249–14253; doi:10.1039/D0RA02673E

data_7240293
_publ_section_title
;
 About the selectivity and reactivity of active nickel electrodes in C--C
 coupling reactions
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              14249
_journal_page_last               14253
_journal_paper_doi               10.1039/D0RA02673E
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C17 H16 Br N O3, C H4 O'
_chemical_formula_sum            'C18 H20 Br N O4'
_chemical_formula_weight         394.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-09 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.574(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.7250(14)
_cell_length_b                   7.9068(3)
_cell_length_c                   15.6809(9)
_cell_measurement_reflns_used    24068
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.66
_cell_volume                     3493.5(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT-2014
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      ' 213 frames, detector distance = 80 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.660
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_T_max  0.7095
_exptl_absorpt_correction_T_min  0.4395
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4172
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0260P)^2^+16.4471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3380
_reflns_number_total             4172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra02673e2.cif
_cod_data_source_block           4d
_cod_depositor_comments          'Adding full bibliography for 7240293.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7240293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.435
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              647