Mono- and dinuclear Ni(i) products formed upon bromide abstraction from the Ni(i) ring-expanded NHC complex [Ni(6-Mes)(PPh<sub>3</sub>)Br].
Blackaby, William J. M.; Sabater, Sara; Poulten, Rebecca C.; Page, Michael J.; Folli, Andrea; Krewald, Vera; Mahon, Mary F.; Murphy, Damien M.; Richards, Emma; Whittlesey, Michael K.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 769–782; doi:10.1039/c7dt04187j

data_7044965
_publ_section_title
;
 Mono- and dinuclear Ni(i) products formed upon bromide abstraction from
 the Ni(i) ring-expanded NHC complex [Ni(6-Mes)(PPh<sub>3</sub>)Br].
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              769
_journal_page_last               782
_journal_paper_doi               10.1039/c7dt04187j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C80 H86 Br N4 Ni2 P2, C32 H12 B F24, C4 H10 O'
_chemical_formula_sum            'C116 H108 B Br F24 N4 Ni2 O P2'
_chemical_formula_weight         2300.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-07 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                75.082(2)
_cell_angle_beta                 84.432(2)
_cell_angle_gamma                87.444(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9050(4)
_cell_length_b                   17.3278(5)
_cell_length_c                   25.2732(6)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.9860
_cell_measurement_theta_min      3.5260
_cell_volume                     5434.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_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_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46948
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.454
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.845
_exptl_crystal_size_mid          0.77
_exptl_crystal_size_min          0.563
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         24033
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0628P)^2^+8.5480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13860
_reflns_number_total             24033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04187j2.cif
_cod_data_source_block           e17mkw42
_cod_depositor_comments
'Adding full bibliography for 7044955--7044965.cif.'
_cod_database_code               7044965
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'orange block'
_shelx_estimated_absorpt_t_max   0.650
_shelx_estimated_absorpt_t_min   0.475
_olex2_refinement_description
;
1. 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
2. Restrained distances
 F15-F14 \\sim F15-F13 \\sim F14-F13 \\sim F13A-F14A \\sim F13A-F15A \\sim
F14A-F15A
 with sigma of 0.02
 C103-F15 \\sim C103-F14 \\sim C103-F13 \\sim C103-F13A \\sim C103-F14A \\sim
C103-F15A
 with sigma of 0.01
 F6A-F5A \\sim F6-F5 \\sim F4-F5 \\sim F5A-F4A \\sim F6A-F4A \\sim F6-F4
 with sigma of 0.02
 C88-F6A \\sim C88-F6 \\sim C88-F4 \\sim C88-F5A \\sim C88-F5 \\sim C88-F4A
 with sigma of 0.01
 F19-F21 \\sim F19-F20 \\sim F21-F20 \\sim F21A-F20A \\sim F21A-F19A \\sim
F20A-F19A
 with sigma of 0.02
 C111-F19 \\sim C111-F21 \\sim C111-F20 \\sim C111-F21A \\sim C111-F20A \\sim
C111-F19A
 with sigma of 0.01
 F2A-F1A \\sim F2A-F3A \\sim F1A-F3A \\sim F2-F3 \\sim F2-F1 \\sim F3-F1
 with sigma of 0.02
 C87A-F2A \\sim C87A-F1A \\sim C87A-F3A \\sim C87-F2 \\sim C87-F3 \\sim C87-F1
 with sigma of 0.01
 C87-C83 \\sim C87A-C83
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(F21A) = Uanis(F21) = Uanis(F20A) = Uanis(F20) = Uanis(F19A) = Uanis(F19)
Uanis(F13) = Uanis(F13A) = Uanis(F15) = Uanis(F15A) = Uanis(F14) = Uanis(F14A)
Uanis(F2) = Uanis(F2A) = Uanis(F1) = Uanis(F1A) = Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F6A) = Uanis(F6) = Uanis(F5A) = Uanis(F5) = Uanis(F4A)
Uanis(C87) = Uanis(C87A)
4. Others
 Fixed Sof: F1(0.65) F2(0.65) F3(0.65) F4(0.65) F5(0.65) F6(0.65) F13(0.55)
 F14(0.55) F15(0.55) F19(0.65) F20(0.65) F21(0.65) F1A(0.35) F2A(0.35)
 F3A(0.35) F4A(0.35) F5A(0.35) F6A(0.35) F13A(0.45) F14A(0.45) F15A(0.45)
 F19A(0.35) F20A(0.35) F21A(0.35) C87(0.65) C87A(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C113(H11D,H11E), C115(H11I,H11J)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), C24(H24), C25(H25), C26(H26), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
  C38(H38), C39(H39), C40(H40), C47(H47), C49(H49), C56(H56), C58(H58),
 C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72),
  C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
 C82(H82), C84(H84), C86(H86), C90(H90), C92(H92), C94(H94), C98(H98),
 C100(H100), C102(H102), C106(H106), C108(H108), C110(H110)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C114(H11F,H11G,H11H), C116(H11K,H11L,H11M)
;