Reactions of the Unsaturated Ditungsten Complexes [W2Cp2(μ-PPh2)2(CO)x] (x = 1, 2) with Nitric Oxide: Stereoselective Carbonyl Displacement and Oxygen-Transfer Reactions of a Nitrite Ligand.
Alvarez, M. Angeles; García, M Esther; García-Vivó, Daniel; Melón, Sonia; Ruiz, Miguel A.; Toyos, Adrián; Inorganic chemistry 53 (2014) 4739–4750; doi:10.1021/ic500498k

data_4338123
_publ_section_title
;
 Reactions of the Unsaturated Ditungsten Complexes [W2Cp2(\m-PPh2)2(CO)x]
 (x = 1, 2) with Nitric Oxide: Stereoselective Carbonyl Displacement and
 Oxygen-Transfer Reactions of a Nitrite Ligand.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4739
_journal_page_last               4750
_journal_paper_doi               10.1021/ic500498k
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H30 N2 O4 P2 W2'
_chemical_formula_sum            'C35 H30 N2 O4 P2 W2'
_chemical_formula_weight         972.25
_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                 121.608(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0876(3)
_cell_length_b                   11.0682(2)
_cell_length_c                   21.9755(6)
_cell_measurement_reflns_used    5904
_cell_measurement_temperature    118(4)
_cell_measurement_theta_max      68.5510
_cell_measurement_theta_min      4.1180
_cell_measurement_wavelength     1.54184
_cell_volume                     3125.35(14)
_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      118(4)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_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  0.041
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12033
_diffrn_reflns_theta_full        68.91
_diffrn_reflns_theta_max         68.91
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    14.73
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.088
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                4880
_reflns_number_total             5635
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500498k_si_002.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 4338123--4338125.cif.'
_cod_database_code               4338123