Stoichiometric and Catalytic Reactivity of Ni(6-Mes)(PPh3)2
Sabater, Sara; Page, Michael J.; Mahon, Mary F.; Whittlesey, Michael K.; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00129

data_4087247
_publ_section_title
;
 Stoichiometric and Catalytic Reactivity of Ni(6-Mes)(PPh3)2
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00129
_journal_year                    2017
_chemical_formula_moiety         'C32 H39 N4 Ni P'
_chemical_formula_sum            'C32 H39 N4 Ni P'
_chemical_formula_weight         569.35
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6104(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.39335(9)
_cell_length_b                   27.1073(2)
_cell_length_c                   13.64061(15)
_cell_measurement_reflns_used    15091
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9580
_cell_measurement_theta_min      3.2410
_cell_volume                     2974.02(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38072
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.167
_diffrn_reflns_theta_min         3.261
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5951
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0324P)^2^+1.2285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5317
_reflns_number_total             5951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bigcif.cif
_cod_data_source_block           s16mkw90
_cod_database_code               4087247
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'yellow tablet'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-C27A \\sim P1-C27
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C27: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim C27A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5)
 C31A(0.5) H31A(0.5) C32A(0.5) H32A(0.5) C27A(0.5) C30(0.5) H30(0.5) C29(0.5)
 H29(0.5) C27(0.5) C32(0.5) H32(0.5) C28(0.5) H28(0.5) C31(0.5) H31(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C28A(H28A), C29A(H29A), C30A(H30A), C31A(H31A),
 C32A(H32A), C30(H30), C29(H29), C32(H32), C28(H28), C31(H31)
5.b Fitted hexagon refined as free rotating group:
 C28A(C29A,C30A,C31A,C32A,C27A)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.490
_oxdiff_exptl_absorpt_empirical_full_min 0.672