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_4338125
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H12 B F24, C34 H30 N O2 P2 W2, C7 H8'
_chemical_formula_sum            'C73 H50 B F24 N O2 P2 W2'
_chemical_formula_weight         1869.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
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_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.575(2)
_cell_angle_beta                 76.783(2)
_cell_angle_gamma                87.726(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7992(4)
_cell_length_b                   14.3171(3)
_cell_length_c                   19.8093(5)
_cell_measurement_reflns_used    21397
_cell_measurement_temperature    139(3)
_cell_measurement_theta_max      69.1980
_cell_measurement_theta_min      3.5300
_cell_measurement_wavelength     1.54184
_cell_volume                     3504.02(16)
_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      139(3)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31075
_diffrn_reflns_theta_full        69.32
_diffrn_reflns_theta_max         69.32
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    7.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42079
_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            orange
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.968
_refine_diff_density_min         -2.477
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         12898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+12.2283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.114
_reflns_number_gt                11729
_reflns_number_total             12898
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500498k_si_002.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 4338123--4338125.cif.'
_cod_database_code               4338125