Arene C(sp(2))-H Metalation at Ni(II) Modeled with a Reactive PONCPh Ligand.
Jongbloed, Linda S.; García-López, Diego; van Heck, Richard; Siegler, Maxime A.; Carbó, Jorge J; van der Vlugt, Jarl Ivar; Inorganic chemistry 55 (2016) 8041–8047; doi:10.1021/acs.inorgchem.6b01162

data_4348412
_publ_section_title
;
 Arene C(sp(2))-H Metalation at Ni(II) Modeled with a Reactive PONCPh
 Ligand.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8041
_journal_page_last               8047
_journal_paper_doi               10.1021/acs.inorgchem.6b01162
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C19 H25 Br N Ni O P'
_chemical_formula_weight         452.99
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.2850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3975(3)
_cell_length_b                   31.1662(10)
_cell_length_c                   12.4348(4)
_cell_measurement_reflns_used    9069
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.7494
_cell_measurement_theta_min      2.8077
_cell_volume                     3921.7(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker ApexII Triumph monochromator sealed tube'
_diffrn_measurement_method       'Photon 50 CMOS detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32507
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.029
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_min         2.810
_exptl_absorpt_coefficient_mu    3.114
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6906
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0333P)^2^+1.0972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4806
_reflns_number_total             6906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01162_si_004.cif
_cod_data_source_block           LSJ_NiPONCBr_3_0m_a_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348412
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.455
_shelx_estimated_absorpt_t_max   0.652
_shelx_res_checksum              77583
_shelx_hkl_checksum              47203