Heterometallic Derivatives of the Unsaturated Ditungsten Hydride [W2(η5-C5H5)2(H)(μ-PCy2)(CO)2]
M. Angeles Alvarez; M. Esther García; Miguel A. Ruiz; Adrián Toyos; M. Fernanda Vega; Inorganic Chemistry 52 (2013) 7068–7077; doi:10.1021/ic400602y

data_4335204
_publ_section_title
;
 Heterometallic Derivatives of the Unsaturated Ditungsten Hydride
 [W2(\h5-C5H5)2(H)(\m-PCy2)(CO)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7068
_journal_page_last               7077
_journal_paper_doi               10.1021/ic400602y
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H33 Fe2 O9 P1 W2'
_chemical_formula_sum            'C31 H33 Fe2 O9 P W2'
_chemical_formula_weight         1059.94
_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_date             2013-04-19
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2955(5)
_cell_length_b                   16.2208(7)
_cell_length_c                   21.1179(11)
_cell_measurement_reflns_used    1983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.70
_cell_measurement_wavelength     0.71073
_cell_volume                     3184.1(3)
_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    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.072
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41478
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    8.198
_exptl_absorpt_correction_T_max  0.7902
_exptl_absorpt_correction_T_min  0.5276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.211
_exptl_crystal_description       needle
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.442
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+19.6710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                4624
_reflns_number_total             6562
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400602y_si_001_2.cif
_cod_data_source_block           compound4
_cod_database_code               4335204