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_4088842
_publ_section_title
;
 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         'C56 H67 N Ni P4, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C57 H69 B2 Cl2 F8 N Ni P4'
_chemical_formula_weight         1195.24
_chemical_name_systematic        '[Ni(8P2N)(dppe)](BF4)2'
_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   geom
_audit_creation_date             2016-01-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                89.347(2)
_cell_angle_beta                 81.996(2)
_cell_angle_gamma                88.173(2)
_cell_formula_units_Z            4
_cell_length_a                   13.1394(6)
_cell_length_b                   19.3197(10)
_cell_length_c                   22.4236(12)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.706
_cell_measurement_theta_min      2.21
_cell_volume                     5633.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            92721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.808
_diffrn_reflns_theta_min         1.393
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0631 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.8356.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             2488
_exptl_crystal_recrystallization_method
'layering hexanes onto a dichloromethane solution.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1458
_refine_ls_number_reflns         28861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+2.9108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22621
_reflns_number_total             28861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00486_si_002.cif
_cod_data_source_block           stol019_0m
_cod_database_code               4088842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(H57C)=Sof(H57D)=Sof(Cl2A)=1-FVAR(1)
 Sof(H57A)=Sof(H57B)=Sof(Cl2)=FVAR(1)
 Sof(F12A)=1-FVAR(2)
 Sof(F12)=FVAR(2)
 Sof(F10A)=1-FVAR(3)
 Sof(F10)=FVAR(3)
 Sof(F3A)=1-FVAR(4)
 Sof(F3)=FVAR(4)
 Sof(F1A)=1-FVAR(5)
 Sof(F1)=FVAR(5)
 Sof(F2A)=1-FVAR(6)
 Sof(F2)=FVAR(6)
 Sof(F4A)=1-FVAR(7)
 Sof(F4)=FVAR(7)
 Sof(H4AB)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C2A)=Sof(H2A)=Sof(C1A)=
 Sof(H1A)=1-FVAR(8)
 Sof(H4AA)=Sof(C3)=Sof(H3)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(H4)=
 FVAR(8)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C19(H19), C25(H25), C6'(H6'), C19'(H19'), C25'(H25')
3.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C5AA(H5AA,H5AB), C5(H5A,
 H5B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C1'(H1'A,H1'B), C2'(H2'A,H2'B),
  C3'(H3'A,H3'B), C4'(H4'A,H4'B), C5'(H5'A,H5'B), C20'(H20C,H20D), C21'(H21C,
 H21D), C22'(H22C,H22D), C23'(H23C,H23D), C24'(H24C,H24D), C26'(H26C,H26D),
 C27'(H27C,H27D), C28'(H28C,H28D), C29'(H29C,H29D), C30'(H30C,H30D), C31'(H31C,
 H31D), C32'(H32C,H32D), C57(H57A,H57B), C57(H57C,H57D), C58(H58A,H58B)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'),
 C12'(H12'), C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'),
 C34'(H34'), C35'(H35'), C36'(H36'), C37'(H37'), C38'(H38'), C40'(H40'),
 C41'(H41'), C42'(H42'), C43'(H43'), C44'(H44'), C46'(H46'), C47'(H47'),
 C48'(H48'), C49'(H49'), C50'(H50'), C52'(H52'), C53'(H53'), C54'(H54'),
 C55'(H55'), C56'(H56'), C4AA(H4AA), C4AA(H4AB), C3(H3), C1(H1), C2(H2), C4(H4),
  C3A(H3A), C4A(H4A), C2A(H2A), C1A(H1A)
;
_shelx_res_checksum              86587
_shelx_hkl_checksum              93920
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'