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_7044963
_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         'C41 H43 N2 Ni O P, F6 P, C4 H8 O'
_chemical_formula_sum            'C45 H51 F6 N2 Ni O2 P2'
_chemical_formula_weight         886.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 95.1450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3080(3)
_cell_length_b                   16.4910(3)
_cell_length_c                   18.8500(4)
_cell_measurement_reflns_used    44246
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      2.910
_cell_volume                     4429.80(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski, Minor 1997)'
_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 0.930
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41528
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.702
_diffrn_reflns_theta_min         3.647
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.051
_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     565
_refine_ls_number_reflns         7457
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0459P)^2^+4.8724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6217
_reflns_number_total             7457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04187j2.cif
_cod_data_source_block           k14mkw21
_cod_depositor_comments
'Adding full bibliography for 7044955--7044965.cif.'
_cod_database_code               7044963
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.894
_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
 F1-F2 \\sim F2-F6 \\sim F6-F5 \\sim F5-F1 \\sim F1A-F2A \\sim F2A-F6A \\sim
F6A-F5A \\sim F5A-F1A
 with sigma of 0.005
 P2-F1 \\sim P2-F2 \\sim P2-F6 \\sim P2-F5 \\sim P2-F1A \\sim P2-F2A \\sim
P2-F6A \\sim P2-F5A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
F2 \\sim F2A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
F6 \\sim F6A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
F5 \\sim F5A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
F1 \\sim F1A: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F5A)
\\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F6) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
4. Others
 Fixed Sof: F1(0.6) F2(0.6) F5(0.6) F6(0.6) F1A(0.4) F2A(0.4) F5A(0.4) F6A(0.4)
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), C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C18(H18), 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)
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)
;
_olex2_submission_special_instructions 'No special instructions were received'