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_4126433
_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_moiety         'C42 H52 N4 Ni2, 0.496(C5 H12)'
_chemical_formula_sum            'C44.48 H57.96 N4 Ni2'
_chemical_formula_weight         766.06
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.4644(7)
_cell_length_b                   37.4644(7)
_cell_length_c                   14.7323(3)
_cell_measurement_reflns_used    98874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.144
_cell_measurement_theta_min      6.251
_cell_volume                     17907.7(6)
_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_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev794 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            98874
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.144
_diffrn_reflns_theta_min         6.251
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_description       rod
_exptl_crystal_F_000             7361
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.000097(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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         7782
_refine_ls_number_restraints     649
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+49.3689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             7782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08691_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        17907.7(8)
_cod_database_code               4126433
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.657
_shelx_estimated_absorpt_t_max   0.858
_shelx_res_checksum              1200
_shelx_hkl_checksum              10655