Transition-Metal Complexes Containing Alkynylsilyl Functionalized η6-Arene Ligands
Hoffmann, Florian; Wagler, Jörg; Roewer, Gerhard; Organometallics 32 (2013) 4531–; doi:10.1021/om400378s

data_4081252
_publ_section_title
;
 Transition-Metal Complexes Containing Alkynylsilyl Functionalized
 \h6-Arene Ligands
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4531
_journal_paper_doi               10.1021/om400378s
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '2(C29 H26 Cr Ni2 O3 Si), 0.5(C10 H8)'
_chemical_formula_sum            'C63 H56 Cr2 Ni4 O6 Si2'
_chemical_formula_weight         1304.02
_chemical_melting_point          383
_chemical_name_common
;
dicyclopentadienyldinickel[phenylethynyldimethylphenylsilane]tricarbonyl-
chromium - 0,25 naphthalene 
;
_chemical_name_systematic
; 
tricarbonyl-1kappa3C-dicyclopentadienyl-2(eta5),3(eta5)-[mu3-dimethyl[phenyl-
1(eta6)](phenylethynyl-2kappa2C,C':3kappa2C,C')silane]-1-chromium(0)-2,3-
bis[nickel(I)](Ni-Ni)-naphthalene (4/1) 
;
_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                97.025(7)
_cell_angle_beta                 104.083(7)
_cell_angle_gamma                105.141(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5160(14)
_cell_length_b                   13.9396(17)
_cell_length_c                   18.172(2)
_cell_measurement_temperature    93(2)
_cell_volume                     2909.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31172
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.9664
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+1.4910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                7523
_reflns_number_total             10286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400378s_si_002.cif
_cod_data_source_block           fh20(compound11*0,25C10H8)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081252