Dehydrogenative Formation and Reactivity of the Unsaturated Benzylidyne-Bridged Complex [Mo2Cp2(μ-CPh)(μ-PCy2)(μ-CO)]: C−C and C−P Coupling Reactions
Alvarez, M. Angeles; García, M. Esther; Martínez, M. Eugenia; Menéndez, Sonia; Ruiz, Miguel A.; Organometallics 29 (2010) 710–; doi:10.1021/om901053x

data_4067636
_publ_section_title
;
 Dehydrogenative Formation and Reactivity of the Unsaturated
 Benzylidyne-Bridged Complex [Mo2Cp2(\m-CPh)(\m-PCy2)(\m-CO)]: C&#x2212;C
 and C&#x2212;P Coupling Reactions
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              710
_journal_paper_doi               10.1021/om901053x
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H39 Cl2 Mo2 O3 P1'
_chemical_formula_sum            'C33 H39 Cl2 Mo2 O3 P'
_chemical_formula_weight         777.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.9990(10)
_cell_angle_beta                 104.2460(10)
_cell_angle_gamma                102.7620(10)
_cell_formula_units_Z            4
_cell_length_a                   10.43100(10)
_cell_length_b                   18.4643(3)
_cell_length_c                   19.0331(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.41
_cell_measurement_wavelength     0.71073
_cell_volume                     3173.12(8)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            170918
_diffrn_reflns_theta_full        33.26
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.8266
_exptl_absorpt_correction_T_min  0.7661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.058
_refine_diff_density_min         -2.34
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         24363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+2.4180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                18634
_reflns_number_total             24363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901053x_si_002.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        3173.12(7)
_cod_database_code               4067636