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_4083075
_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         'C36 H38 N4 Ni P2, 2(C24 H20 B)'
_chemical_formula_sum            'C84 H78 B2 N4 Ni P2'
_chemical_formula_weight         1285.77
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-19
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.11.06 svn.r2526, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.611(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.5248(7)
_cell_length_b                   14.3650(4)
_cell_length_c                   20.1176(6)
_cell_measurement_reflns_used    8726
_cell_measurement_temperature    140
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.50
_cell_volume                     6791.6(3)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      140.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78476
_diffrn_reflns_theta_full        29.74
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         0.87
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0727 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.9255.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         19167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+1.9247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                12363
_reflns_number_total             19167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500206e_si_003.cif
_cod_data_source_block           Ni-PPh2
_cod_depositor_comments
'Adding full bibliography for 4083074--4083076.cif.'
_cod_database_code               4083075
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, H6 of C6, H2 of C2, H8 of C8, H21 of C21, H3 of C3, H4 of C4, H44
  of C44, {H32A,H32B} of C32, H34 of C34, H35 of C35, H38 of C38, H39 of C39,
  H40 of C40, H41 of C41, H42 of C42, H26 of C26, H27 of C27, H22 of C22, H23
  of C23, H24 of C24, H28 of C28, H20 of C20, H29 of C29, H30 of C30, H45 of
  C45, H46 of C46, H47 of C47, H50 of C50, H51 of C51, H52 of C52, H53 of C53,
  H54 of C54, H56 of C56, H57 of C57, H58 of C58, H59 of C59, H60 of C60, H62
  of C62, H63 of C63, H64 of C64, H65 of C65, H66 of C66, H68 of C68, H69 of
  C69, H70 of C70, H71 of C71, H72 of C72, H74 of C74, H75 of C75, H76 of C76,
  H77 of C77, H78 of C78, H80 of C80, H81 of C81, H82 of C82, H83 of C83, H84
  of C84, H48 of C48, {H31A,H31B} of C31, H9 of C9, H10 of C10, H11 of C11, H12
  of C12, {H13A,H13B} of C13, {H14A,H14B} of C14, H16 of C16, H17 of C17
 At 1.5 times of:
  {H36A,H36B,H36C} of C36, {H18A,H18B,H18C} of C18
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C31(H31A,H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
 C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80), C81(H81), C82(H82),
  C83(H83), C84(H84)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C36(H36A,H36B,H36C)
;