Catalytic Oxidation of Alcohol via Nickel Phosphine Complexes with Pendant Amines
Weiss, Charles J.; Das, Parthapratim; Miller, Deanna L.; Helm, Monte L.; Appel, Aaron M.; ACS Catalysis 4 (2014) 2951–; doi:10.1021/cs500853f

data_4511783
_publ_section_title
;
 Catalytic Oxidation of Alcohol via Nickel Phosphine Complexes with
 Pendant Amines
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              2951
_journal_paper_doi               10.1021/cs500853f
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C24 H50 N4 Ni P2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C26 H53 B2 F8 N5 Ni P2'
_chemical_formula_weight         730.00
_chemical_name_systematic        '[Ni(PtBu2NtBu2)(CH3CN)2](BF4)2'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4813)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.393(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6454(9)
_cell_length_b                   10.5867(9)
_cell_length_c                   17.3734(15)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    140
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      2.24
_cell_volume                     1957.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40144
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.772
_diffrn_reflns_theta_min         1.172
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1201 before and 0.0752 after correction.
The Ratio of minimum to maximum transmission is 0.7979.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.118
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         11845
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0766
_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^)+(0.1015P)^2^+6.0211P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2093
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                10551
_reflns_number_total             11845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs500853f_si_002.cif
_cod_data_source_block           helm155_0m
_cod_depositor_comments
'Adding full bibliography for 4511782--4511784.cif.'
_cod_database_code               4511783
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.709
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C25) = Uanis(C26)
3. Others
 Sof(F4A)=Sof(F2A)=1-FVAR(1)
 Sof(F2)=Sof(F4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              98615
_shelx_hkl_checksum              63718