Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis of H2
Stolley, Ryan M.; Darmon, Jonathan M.; Das, Parthapratim; Helm, Monte L.; Organometallics 35 (2016) 2965–; doi:10.1021/acs.organomet.6b00486

data_4088845
_publ_section_title
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 Nickel Bis-Diphosphine Complexes: Controlling the Binding and Heterolysis
 of H2
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2965
_journal_paper_doi               10.1021/acs.organomet.6b00486
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C43 H59 N Ni P4, 2(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C45 H63 B2 Cl4 F8 N Ni P4'
_chemical_formula_weight         1115.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                99.581(3)
_cell_angle_beta                 91.152(3)
_cell_angle_gamma                100.361(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6309(8)
_cell_length_b                   12.6929(9)
_cell_length_c                   20.0253(14)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.41
_cell_volume                     2617.5(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., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.832
_diffrn_reflns_theta_min         1.033
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.758
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0589 before and 0.0431 after correction.
The Ratio of minimum to maximum transmission is 0.8527.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.558
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.093
_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     648
_refine_ls_number_reflns         13486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+4.5083P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10583
_reflns_number_total             13486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00486_si_002.cif
_cod_data_source_block           xprep2
_cod_database_code               4088845
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Others
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C17A)=Sof(H17C)=
 Sof(H17D)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=1-FVAR(2)
 Sof(C15A)=Sof(H15C)=Sof(H15D)=FVAR(2)
 Sof(C16)=Sof(H16A)=Sof(H16B)=1-FVAR(3)
 Sof(C16A)=Sof(H16C)=Sof(H16D)=FVAR(3)
 Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(4)
 Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C12A(H12A)
3.b Secondary CH2 refined with riding coordinates:
 N1(H2,H3), C1(H1C,H1D), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C42(H42A,H42B), C43(H43A,H43B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C13A(H13C,H13D), C14A(H14C,H14D), C15A(H15C,
 H15D), C16A(H16C,H16D), C17A(H17C,H17D), C44(H44A,H44B), C45(H45A,H45B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              97426
_shelx_hkl_checksum              84826
_olex2_submission_special_instructions 'No special instructions were received'