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_4334341
_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         'C32 H39 N1 O5 P1 Re1 W2'
_chemical_formula_sum            'C32 H39 N O5 P Re W2'
_chemical_formula_weight         1102.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 113.516(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.5058(19)
_cell_length_b                   11.0077(4)
_cell_length_c                   17.6403(9)
_cell_measurement_reflns_used    5003
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5360
_cell_measurement_theta_min      2.9833
_cell_measurement_wavelength     1.54184
_cell_volume                     6321.9(6)
_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      150.00(10)
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.96
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11390
_diffrn_reflns_theta_full        72.69
_diffrn_reflns_theta_max         72.69
_diffrn_reflns_theta_min         4.24
_exptl_absorpt_coefficient_mu    21.294
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_description       needle
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.622
_refine_diff_density_min         -3.311
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       0.000056(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0522
_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^)+(0.1081P)^2^+16.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.15
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                5217
_reflns_number_total             6032
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic3027489_si_001_2.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        6321.9(5)
_cod_database_code               4334341