Low-Temperature N-O Bond Cleavage and Reversible N-P Bond Formation Processes in the Reactions of the Unsaturated Anions [M2(η5-C5H5)2(μ-PCy2)(μ-CO)2]- (M = Mo, W) with the Nitrosyl Complex [Re(η5-C5H4Me)(CO)2(NO)]+
M. Angeles Alvarez; M. Esther García; Miguel A. Ruiz; Adrián Toyos; M. Fernanda Vega; Inorganic Chemistry 52 (2013) 3942–3952; doi:10.1021/ic3027489

data_4334342
_publ_section_title
;
 Low-Temperature N-O Bond Cleavage and Reversible N-P Bond Formation
 Processes in the Reactions of the Unsaturated Anions
 [M2(\h5-C5H5)2(\m-PCy2)(\m-CO)2]- (M = Mo, W) with the Nitrosyl Complex
 [Re(\h5-C5H4Me)(CO)2(NO)]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3942
_journal_page_last               3952
_journal_paper_doi               10.1021/ic3027489
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C53 H71 N2 O5 P2 Re W4'
_chemical_formula_sum            'C53 H71 N2 O5 P2 Re W4'
_chemical_formula_weight         1799.63
_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      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.911(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8430(8)
_cell_length_b                   22.4890(9)
_cell_length_c                   15.6359(6)
_cell_measurement_reflns_used    6705
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.8138
_cell_measurement_theta_min      2.8757
_cell_measurement_wavelength     1.54184
_cell_volume                     5815.5(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20703
_diffrn_reflns_theta_full        73.98
_diffrn_reflns_theta_max         73.98
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    19.041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_description       prism
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         2.591
_refine_diff_density_min         -2.877
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11283
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.173
_reflns_number_gt                9410
_reflns_number_total             11283
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3027489_si_001_3.cif
_cod_data_source_block           compound8
_cod_database_code               4334342