Dimolybdenum Cyclopentadienyl Complexes with Bridging Chalcogenophosphinidene Ligands
Belén Alvarez; M. Angeles Alvarez; Inmaculada Amor; M. Esther García; Daniel García-Vivó; Jaime Suárez; Miguel A. Ruiz; Inorganic Chemistry 51 (2012) 7810–7824; doi:10.1021/ic300869z

data_4329733
_publ_section_title
;
 Dimolybdenum Cyclopentadienyl Complexes with Bridging
 Chalcogenophosphinidene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7810
_journal_page_last               7824
_journal_paper_doi               10.1021/ic300869z
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H48 Mo2 N1 O2 P1 S1'
_chemical_formula_sum            'C35 H48 Mo2 N O2 P S'
_chemical_formula_weight         769.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.066(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   17.154(5)
_cell_length_b                   11.003(5)
_cell_length_c                   18.268(5)
_cell_measurement_reflns_used    1826
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      26.1705
_cell_measurement_theta_min      2.2295
_cell_measurement_wavelength     0.71073
_cell_volume                     3448(2)
_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, 2008)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.022
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            67491
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+12.2848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                5773
_reflns_number_total             6792
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic300869z_si_002_6.cif
_cod_data_source_block           syn10b
_cod_database_code               4329733