Reactions of Cp2M (M = Ni, V) with dilithium diamido-aryl reagents; retention and oxidation of the transition metal ions.
Stokes, Francesca A.; Vincent, Mark A.; Hillier, Ian H.; Ronson, Tanya K.; Steiner, Alexander; Wheatley, Andrew E. H.; Wood, Paul T.; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13923–13930; doi:10.1039/c3dt51632f

data_7021940
_publ_section_title
;
 Reactions of Cp2M (M = Ni, V) with dilithium diamido-aryl reagents;
 retention and oxidation of the transition metal ions.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13923
_journal_page_last               13930
_journal_paper_doi               10.1039/c3dt51632f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety
; 
 'C36 H36 N12 Ni6, C40 H41 Li N12 O Ni6 2-,
  2(C16 H32 Li O4 1+), 5(C4 H8 O)'
;
_chemical_formula_sum            'C128 H181 Li3 N24 Ni12 O14'
_chemical_formula_weight         3005.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.948(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   13.2275(3)
_cell_length_b                   17.0537(7)
_cell_length_c                   16.5692(6)
_cell_volume                     3717.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Beamline I19, Diamond Light Source'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27906
_diffrn_reflns_theta_full        22.75
_diffrn_reflns_theta_max         22.75
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.46(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         10066
_refine_ls_number_restraints     1070
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.2344
_refine_ls_R_factor_gt           0.1384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3256
_refine_ls_wR_factor_ref         0.3662
_reflns_number_gt                4604
_reflns_number_total             10066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51632f.txt
_cod_data_source_block           p21
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7021940