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_4329732
_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         'C32 H41 Cl2 Mo2 O3 P1 Se1'
_chemical_formula_sum            'C32 H41 Cl2 Mo2 O3 P Se'
_chemical_formula_weight         846.36
_chemical_name_systematic
;
 ?
;
_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      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.242(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.54060(10)
_cell_length_b                   16.6907(2)
_cell_length_c                   19.3623(2)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     3352.13(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            42521
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.84304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.913
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+3.0288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                5171
_reflns_number_total             6020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300869z_si_002_5.cif
_cod_data_source_block           syn8c
_cod_original_cell_volume        3352.13(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329732