Displacement of η<sup>5</sup>-cyclopentadienyl ligands from half-sandwich C,C-(NHC-cyanoalkyl)-nickel(ii) metallacycles: further insight into the structure of the resulting Cp-free nickelacycles and a catalytic activity study.
Cardoso, Bernardo de P; Bernard-Schaaf, Jean-Marie; Shahane, Saurabh; Veiros, Luis F.; Chetcuti, Michael J.; Ritleng, Vincent; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1535–1547; doi:10.1039/c7dt04560c

data_7045150
_publ_section_title
;
 Displacement of \h<sup>5</sup>-cyclopentadienyl ligands from
 half-sandwich C,C-(NHC-cyanoalkyl)-nickel(ii) metallacycles: further
 insight into the structure of the resulting Cp-free nickelacycles and a
 catalytic activity study.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1535
_journal_page_last               1547
_journal_paper_doi               10.1039/c7dt04560c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H21 N3 Ni'
_chemical_formula_sum            'C20 H21 N3 Ni'
_chemical_formula_weight         362.11
_chemical_properties_physical    Air-sensitive
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-11-16 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                80.591(6)
_cell_angle_beta                 86.833(7)
_cell_angle_gamma                82.101(7)
_cell_formula_units_Z            4
_cell_length_a                   9.3425(10)
_cell_length_b                   13.7491(15)
_cell_length_c                   14.2032(15)
_cell_measurement_reflns_used    7379
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.39
_cell_measurement_theta_min      5.44
_cell_volume                     1781.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27037
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.104
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0883
_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^)+(0.1380P)^2^+4.0164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.2721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4232
_reflns_number_total             6205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04560c2.cif
_cod_data_source_block           mcbc161020
_cod_depositor_comments
'Adding full bibliography for 7045149--7045150.cif.'
_cod_database_code               7045150
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.911
_shelxl_version_number           2013-4
_shelx_res_checksum              69007