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_1564899
_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            'C52 H40 Cl2 Fe N2 Ni2 P2'
_chemical_formula_weight         998.97
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
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_cell_angle_gamma                90
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_cell_length_b                   10.33270(10)
_cell_length_c                   18.9251(3)
_cell_measurement_reflns_used    18200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.5400
_cell_measurement_theta_min      2.4150
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_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_publication_material  'SHELXL in WINGX'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Synergy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         72.764
_diffrn_reflns_theta_min         3.989
_diffrn_source                   'microsource tube'
_exptl_absorpt_coefficient_mu    5.797
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4296
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0683P)^2^+7.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             4296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04582b3.cif
_cod_data_source_block           1clquin_nidimer
_cod_original_cell_volume        4333.63(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1564899
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              34661
_shelx_hkl_checksum              85841