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_4088841
_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         'C60 H86 N2 Ni P4, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C62 H89 B2 F8 N3 Ni P4'
_chemical_formula_weight         1232.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P -2bc -2c'
_space_group_name_H-M_alt        'P c 21 b'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7934(4)
_cell_length_b                   23.4534(8)
_cell_length_c                   26.9825(10)
_cell_measurement_reflns_used    8191
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.21
_cell_volume                     6197.6(4)
_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      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27105
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         1.737
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0658 before and 0.0390 after correction.
The Ratio of minimum to maximum transmission is 0.8535.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 4606 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         12235
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0705P)^2^+1.9278P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10844
_reflns_number_total             12235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00486_si_002.cif
_cod_data_source_block           ee33pd_0m
_cod_database_code               4088841
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.530(16) 0.470(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C18(H18), C36(H36), C42(H42), C48(H48)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), 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), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
3.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C)
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_shelx_res_checksum              74460
_shelx_hkl_checksum              51305
_olex2_submission_special_instructions 'No special instructions were received'