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_7044962
_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 H46 B N3 Ni P, C4 H8 O'
_chemical_formula_sum            'C45 H54 B N3 Ni O P'
_chemical_formula_weight         753.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-12
_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                 108.838(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2120(4)
_cell_length_b                   16.5650(4)
_cell_length_c                   18.0386(6)
_cell_measurement_reflns_used    8369
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.8540
_cell_measurement_theta_min      3.7710
_cell_volume                     4019.2(2)
_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_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38736
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.407
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83441
_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            pale-yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.621
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9218
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0552P)^2^+3.9228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6952
_reflns_number_total             9218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04187j2.cif
_cod_data_source_block           e17mkw37
_cod_depositor_comments
'Adding full bibliography for 7044955--7044965.cif.'
_cod_database_code               7044962
_shelxl_version_number           2014-3
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C43 \\sim C43-C42
 with sigma of 0.005
 O1-C45 \\sim O1A-C45 \\sim O1A-C42 \\sim O1-C42
 with sigma of 0.005
 C44-C43 \\sim C44A-C43 \\sim C45-C44 \\sim C45-C44A
 with sigma of 0.005
 C4-C3A \\sim C4-C3 \\sim C3A-C2 \\sim C3-C2
 with sigma of 0.005
 B1-H1A \\sim B1-H1C \\sim B1-H1B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) = Uanis(O1)
Uanis(C44A) = Uanis(C44)
4. Others
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5) H4AA(0.5) H4AB(0.5)
 H4BC(0.5) H4BD(0.5) C3(0.5) H3A(0.5) H3B(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5)
 O1(0.75) O1A(0.25) H42A(0.75) H42B(0.75) H42C(0.25) H42D(0.25) H43A(0.75)
 H43B(0.75) H43C(0.25) H43D(0.25) H45A(0.75) H45B(0.75) H45C(0.25) H45D(0.25)
 C44(0.75) H44A(0.75) H44B(0.75) C44A(0.25) H44C(0.25) H44D(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C4(H4AA,H4AB), C4(H4BC,H4BD), C3(H3A,H3B),
 C3A(H3AA,H3AB), C42(H42A,H42B), C42(H42C,H42D), C43(H43A,H43B), C43(H43C,H43D),
  C45(H45A,H45B), C45(H45C,H45D), C44(H44A,H44B), C44A(H44C,H44D)
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'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;