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_4348403
_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 H26 B Br F4 N Ni O P'
_chemical_formula_weight         540.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8324(5)
_cell_length_b                   12.7020(8)
_cell_length_c                   22.4682(15)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.987
_cell_measurement_theta_min      2.754
_cell_volume                     2235.3(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.997
_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  0.0666
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37723
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.754
_exptl_absorpt_coefficient_mu    2.770
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       needle
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.708
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.35(2)
_refine_ls_extinction_coef       0.0042(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3932
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+8.1642P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3602
_reflns_number_total             3932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01162_si_003.cif
_cod_data_source_block           lsj
_cod_database_code               4348403
_shelx_estimated_absorpt_t_min   0.490
_shelx_estimated_absorpt_t_max   0.681
_shelxl_version_number           2013-2
_shelx_res_checksum              45687
_shelx_hkl_checksum              52046