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_7044961
_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         '2(C31 H40 N2 Ni), 2(B C24 F20)'
_chemical_formula_sum            'C110 H80.2 B2 F40 N4 Ni1.8'
_chemical_formula_weight         2345.27
_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     direct
_audit_creation_date             2017-10-03
_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                92.241(3)
_cell_angle_beta                 90.291(3)
_cell_angle_gamma                107.737(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4000(4)
_cell_length_b                   16.7387(6)
_cell_length_c                   29.4479(9)
_cell_measurement_reflns_used    8992
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.3070
_cell_measurement_theta_min      4.5100
_cell_volume                     4878.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31281
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.099
_diffrn_reflns_theta_min         4.509
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabloid
_exptl_crystal_F_000             2377
_exptl_crystal_size_max          0.2234
_exptl_crystal_size_mid          0.1027
_exptl_crystal_size_min          0.0374
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1525
_refine_ls_number_reflns         18573
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0890
_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^)+(0.1357P)^2^+5.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2431
_refine_ls_wR_factor_ref         0.2676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13518
_reflns_number_total             18573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04187j2.cif
_cod_data_source_block           s14mkw3
_cod_depositor_comments
'Adding full bibliography for 7044955--7044965.cif.'
_cod_original_formula_sum        'C110 H80.20 B2 F40 N4 Ni1.80'
_cod_database_code               7044961
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.715
_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
 B1-C63 \\sim B1A-C63A
 with sigma of 0.005
 F1-B1 \\sim F1A-B1
 with sigma of 0.005
 C32-Ni2 \\sim C32-Ni2A
 with sigma of 0.02
 C1-Ni1 \\sim C1-Ni1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4A)
\\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(C63A) \\sim Ueq, Uanis(C64A) \\sim Ueq,
Uanis(C65A) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C68A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B1) = Uanis(B1A)
Uanis(Ni1) = Uanis(Ni1A)
Uanis(Ni2) = Uanis(Ni2A)
4. Others
 Fixed Sof: Ni1(0.85) Ni1A(0.15) Ni2(0.75) Ni2A(0.05) F1(0.65) F2(0.65)
 F3(0.65) F4(0.65) F5(0.65) F1A(0.35) F2A(0.35) F3A(0.35) F4A(0.35) F5A(0.35)
 C63(0.65) C64(0.65) C65(0.65) C66(0.65) C67(0.65) C68(0.65) C63A(0.35)
 C64A(0.35) C65A(0.35) C66A(0.35) C67A(0.35) C68A(0.35) B1(0.65) B1A(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), C23(H23), C25(H25), C27(H27), C38(H38),
 C40(H40), C47(H47), C49(H49), C54(H54), C56(H56), C58(H58)
5.c Fitted hexagon refined as free rotating group:
 C63(C64,C65,C66,C67,C68), C63A(C64A,C65A,C66A,C67A,C68A)
5.d 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), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_olex2_submission_special_instructions 'No special instructions were received'