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

data_4081253
_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         'C33 H26 Mo3 O7 Si'
_chemical_formula_sum            'C33 H26 Mo3 O7 Si'
_chemical_formula_weight         850.45
_chemical_melting_point          498
_chemical_name_common
;
tetracarbonyldicyclopentadienyldimolybdenum[phenylethynyldimethylphenylsilane]-
tricarbonylmolybdenum 
;
_chemical_name_systematic
; 
heptacarbonyl-1kappa3C,2kappa2C,3kappa2C-dicyclopentadienyl-2(eta5),3(eta5)-
[mu3-dimethyl[phenyl-1(eta6)](phenylethynyl-2kappa2C,C':3kappa2C,C')silane]-
1-molybdenum(0)-2,3-bis[molybdenum(I)](Mo2-Mo3) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.863(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8575(10)
_cell_length_b                   11.3366(8)
_cell_length_c                   15.0233(10)
_cell_measurement_temperature    93(2)
_cell_volume                     3118.1(3)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.1331
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7568
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5468
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                3714
_reflns_number_total             5468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400378s_si_002.cif
_cod_data_source_block           fh24(compound12)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4081253