Nickel-Catalyzed Decarbonylation of N-Acylated N-Heteroarenes
Tobisu, Mamoru; Morioka, Toshifumi; Nakatani, Syun; Sakamoto, Yuki; Kodama, Takuya; Ogoshi, Sensuke; Chatani, Naoto; Chemical Science  (2019) –; doi:10.1039/C9SC02035G

data_1551170
_publ_section_title
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 Nickel-Catalyzed Decarbonylation of N-Acylated N-Heteroarenes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02035G
_journal_year                    2019
_chemical_formula_moiety         'C41 H54 F3 N Ni P2'
_chemical_formula_sum            'C41 H54 F3 N Ni P2'
_chemical_formula_weight         738.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-03-07 deposited with the CCDC.    2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.787(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   16.8932(6)
_cell_length_b                   36.2820(11)
_cell_length_c                   13.0079(5)
_cell_measurement_reflns_used    20774
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.88
_cell_measurement_theta_min      2.13
_cell_volume                     7743.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            73717
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        31.140
_diffrn_reflns_theta_max         31.140
_diffrn_reflns_theta_min         1.871
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nONE
_exptl_crystal_F_000             3136.00
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.182
_refine_diff_density_max         1.10
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     899
_refine_ls_number_reflns         19566
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0881P)^2^+16.0760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                13491
_reflns_number_total             19566
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9sc02035g2.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C82 H108 F6 N2 Ni2 P4'
_cod_original_formula_weight         1477.05
_cod_original_formula_moiety         'C82 H108 F6 N2 Ni2 P4'
_cod_original_formula_units_Z            4
_cod_database_code               1551170