Inhibition of (dppf)nickel-catalysed Suzuki-Miyaura cross-coupling reactions by α-halo-N-heterocycles
Cooper, Alasdair K.; Greaves, Megan E.; Donohoe, William; Burton, Paul Matthew; Ronson, Thomas Oliver; Kennedy, Alan; Nelson, David James; Chemical Science  (2021) –; doi:10.1039/D1SC04582B

data_1564897
_publ_section_title
;
 Inhibition of (dppf)nickel-catalysed Suzuki-Miyaura cross-coupling
 reactions by \a-halo-N-heterocycles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04582B
_journal_year                    2021
_chemical_formula_sum            'C46 H40 Br2 Cl4 Fe N2 Ni2 P2'
_chemical_formula_weight         1157.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.5400(10)
_cell_angle_gamma                90
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_cell_length_b                   17.1989(2)
_cell_length_c                   20.6947(2)
_cell_measurement_reflns_used    12934
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_cell_measurement_theta_max      73.0610
_cell_measurement_theta_min      3.3730
_cell_volume                     4504.60(8)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34815
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.105
_diffrn_reflns_theta_min         3.348
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.733
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       'fragment cut from large prism'
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8918
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0815P)^2^+4.5018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7957
_reflns_number_total             8918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04582b3.cif
_cod_data_source_block           nelson_ac_oct2020
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1564897
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              22084
_shelx_hkl_checksum              15585