Synthesis, Redox Chemistry, and Electronic Structure of the Alkynyl Cyclopentadienyl Molybdenum Complexes [Mo(C\τb CR)(CO)(L2)Cp′]n+(n= 0 or 1; R = Ph or C6H4-4-Me, L2= Ph2PCH2CH2PPh2or 2PMe3, Cp′ = Cp or Cp*)
Roberts (née Lancashire), Hannah N.; Brown, Neil J.; Edge, Ruth; Lewin, Ross; Collison, David; Low, Paul J.; Whiteley, Mark W.; Organometallics 30 (2011) 3763–; doi:10.1021/om200229c

data_4064627
_publ_contact_author
; 
    Hannah Roberts
;
_publ_section_title
;
 Synthesis, Redox Chemistry, and Electronic Structure of the Alkynyl
 Cyclopentadienyl Molybdenum Complexes [Mo(C\\tb
 CR)(CO)(L2)Cp&#x2032;]n+(n= 0 or 1; R = Ph or C6H4-4-Me, L2=
 Ph2PCH2CH2PPh2or 2PMe3, Cp&#x2032; = Cp or Cp*)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3763
_journal_paper_doi               10.1021/om200229c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C45 H44 Mo O P2'
_chemical_formula_sum            'C45 H44 Mo O P2'
_chemical_formula_weight         758.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.170(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9199(3)
_cell_length_b                   21.3484(7)
_cell_length_c                   17.4064(6)
_cell_measurement_reflns_used    7893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6293
_cell_measurement_theta_min      2.8572
_cell_volume                     3603.4(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.9087
_exptl_absorpt_correction_T_min  0.9087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0699
_reflns_number_gt                5313
_reflns_number_total             8203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200229c_si_002.cif
_cod_data_source_block           omww56
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064627