Facile displacement of eta^5^-cyclopentadienyl ligands from half-sandwich alkyl, NHC-nickel complexes: an original route to robust cis-C,C-nickel square planar complexes
Mickael Henrion; Anna Magdalena Oertel; Vincent Ritleng; Michael J. Chetcuti; Chem.Commun. 49 (2013) 6424–; doi:10.1039/c3cc43691h

data_7109484
_publ_section_title
;
 Facile displacement of eta^5^-cyclopentadienyl ligands from half-sandwich
 alkyl, NHC-nickel complexes: an original route to robust cis-C,C-nickel
 square planar complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              6424
_journal_paper_doi               10.1039/c3cc43691h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C21 H25 N3 Ni O2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C23 H29 N3 Ni O2.5'
_chemical_formula_weight         446.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4575(4)
_cell_length_b                   18.4575(4)
_cell_length_c                   13.1542(4)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.91
_cell_volume                     4481.36(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29009
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_correction_T_min  0.8419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+1.8706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                4775
_reflns_number_total             5149
_reflns_threshold_expression     I>2sigma(I)
_cod_depositor_comments
;

2018-11-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C46 H58 N6 Ni2 O5'
_cod_original_formula_weight         892.40
_cod_original_formula_moiety         '2(C21 H25 N3 Ni O2), C4 H8 O'
_cod_original_formula_units_Z            4
_cod_data_source_file            c3cc43691h.txt
_cod_data_source_block           mcamo100310_02
_cod_database_code               7109484