Catalytic Carbonylative Rearrangement of Norbornadiene via Dinuclear Carbon-Carbon Oxidative Addition.
Hartline, Douglas R.; Zeller, Matthias; Uyeda, Christopher; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08691

data_4126434
_publ_section_title
;
 Catalytic Carbonylative Rearrangement of Norbornadiene via Dinuclear
 Carbon-Carbon Oxidative Addition.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08691
_journal_year                    2017
_chemical_formula_sum            'C43 H52 N4 Ni2'
_chemical_formula_weight         742.30
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 100.0431(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9528(2)
_cell_length_b                   20.2181(4)
_cell_length_c                   14.3665(3)
_cell_measurement_reflns_used    72104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.299
_cell_measurement_theta_min      5.058
_cell_volume                     3704.66(12)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'Encifer (Allen et al., 2004)'
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2017), 
SHELXLE Rev761 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72104
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.299
_diffrn_reflns_theta_min         5.058
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00135(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0606P)^2^+7.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7082
_reflns_number_total             7233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08691_si_001.cif
_cod_data_source_block           3
_cod_database_code               4126434
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.516
_shelx_estimated_absorpt_t_max   0.618
_shelx_res_checksum              57074
_shelx_hkl_checksum              73491