Monomeric Alkoxo and Amido Methylnickel(II) Complexes. Synthesis and Heterocumulene Insertion Chemistry
Cámpora, Juan; Matas, Inmaculada; Palma, Pilar; Álvarez, Eleuterio; Graiff, Claudia; Tiripicchio, Antonio; Organometallics 26 (2007) 3840–; doi:10.1021/om7002909

data_4073363
_publ_section_title
;
 Monomeric Alkoxo and Amido Methylnickel(II) Complexes. Synthesis and
 Heterocumulene Insertion Chemistry
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3840
_journal_paper_doi               10.1021/om7002909
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C26 H48 N2 Ni P2 S'
_chemical_formula_sum            'C26 H48 N2 Ni P2 S'
_chemical_formula_weight         541.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                100.194(2)
_cell_angle_beta                 93.297(2)
_cell_angle_gamma                99.191(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3613(16)
_cell_length_b                   10.3787(16)
_cell_length_c                   14.333(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2
_cell_volume                     1491.7(4)
_computing_cell_refinement       'Software SMART Bruker'
_computing_data_collection       'Software SMART Bruker'
_computing_data_reduction        'SAINT Bruker'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker AXS SMART 1000'
_diffrn_measurement_method       'omega scan'
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15881
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS: Area-Detector Absorption Correction. Bruker-AXS
  within v. 7.06 a (Bruker AXS, 2003).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6955
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1312P)^2^+1.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.2087
_reflns_number_gt                4355
_reflns_number_total             6955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7002909-file001.cif
_cod_data_source_block           19
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073363