Structure and dynamics of heterometallic clusters derived from addition of metal carbonyl fragments to the unsaturated hydride [W2Cp2(μ-H)(μ-PPh2)(NO)2]
Angeles Alvarez, M.; Esther García, M.; García-Vivó, Daniel; Ruiz, Miguel A.; Toyos, Adrián; Dalton Trans.  (2017) –; doi:10.1039/C7DT03580B

data_7044542
_publ_section_title
;
 Structure and dynamics of heterometallic clusters derived from addition
 of metal carbonyl fragments to the unsaturated hydride
 [W2Cp2(\m-H)(\m-PPh2)(NO)2]
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03580B
_journal_year                    2017
_chemical_formula_moiety         'C27 H21 N2 O7 P W3'
_chemical_formula_sum            'C27 H21 N2 O7 P W3'
_chemical_formula_weight         1067.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016
_audit_update_record
;
2017-07-31 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                102.888(4)
_cell_angle_beta                 93.925(4)
_cell_angle_gamma                94.326(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0754(5)
_cell_length_b                   10.9594(6)
_cell_length_c                   14.9036(6)
_cell_measurement_reflns_used    6729
_cell_measurement_temperature    155(4)
_cell_measurement_theta_max      69.6170
_cell_measurement_theta_min      4.1550
_cell_volume                     1435.31(13)
_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 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      155(4)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.963
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9911
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.743
_diffrn_reflns_theta_min         4.156
_exptl_absorpt_coefficient_mu    22.670
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             980
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichoromethane/toluene/petroleum ether'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         10.010
_refine_diff_density_min         -4.073
_refine_diff_density_rms         0.690
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5205
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4446
_reflns_number_total             5205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03580b3.cif
_cod_data_source_block           compound3
_cod_database_code               7044542
_shelx_res_checksum              67825