Effects of Phosphine–Carbene Substitutions on the Electrochemical and Thermodynamic Properties of Nickel Complexes
Galan, Brandon R.; Wiedner, Eric S.; Helm, Monte L.; Linehan, John C.; Appel, Aaron M.; Organometallics 33 (2014) 2287–; doi:10.1021/om500206e

data_4083074
_publ_section_title
;
 Effects of Phosphine--Carbene Substitutions on the Electrochemical and
 Thermodynamic Properties of Nickel Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2287
_journal_paper_doi               10.1021/om500206e
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C24 H20 B, C6 H10 Cl N2'
_chemical_formula_sum            'C30 H30 B Cl N2'
_chemical_formula_weight         464.82
_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_date             2013-02-19
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.11.06 svn.r2526, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.659(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2046(8)
_cell_length_b                   20.1274(19)
_cell_length_c                   12.3318(12)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      32.091
_cell_measurement_theta_min      2.538
_cell_volume                     2530.1(4)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      140.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38988
_diffrn_reflns_theta_full        32.15
_diffrn_reflns_theta_max         32.15
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0765 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.8732.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         8827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.6290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                6785
_reflns_number_total             8827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500206e_si_003.cif
_cod_data_source_block           helm142_0m
_cod_depositor_comments
'Adding full bibliography for 4083074--4083076.cif.'
_cod_database_code               4083074
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H23 of C23, H24 of C24, {H5A,H5B} of C5, H9 of C9, H10 of C10, H8 of C8,
  H27 of C27, H3 of C3, H11 of C11, H12 of C12, H14 of C14, H15 of C15, H16 of
  C16, H17 of C17, H18 of C18, H20 of C20, H21 of C21, {H6A,H6B} of C6, H2 of
  C2, H22 of C22, H28 of C28, H29 of C29, H30 of C30, H26 of C26
 At 1.5 times of:
  {H4A,H4B,H4C} of C4
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;