Thermally Stable Diazoalkane Derivatives of the Unsaturated Ditungsten Hydride [W2Cp2(H)(μ-PCy2)(CO)2]
Alvarez, M. Angeles; García, M. Esther; García-Vivó, Daniel; Huergo, Estefanía; Ruiz, Miguel A.; Vega, M. Fernanda; Organometallics 34 (2015) 3833–; doi:10.1021/acs.organomet.5b00466

data_4086096
_publ_section_title
;
 Thermally Stable Diazoalkane Derivatives of the Unsaturated Ditungsten
 Hydride [W2Cp2(H)(\m-PCy2)(CO)2]
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3833
_journal_paper_doi               10.1021/acs.organomet.5b00466
_journal_volume                  34
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C50 H53 N4 O2 P W2'
_chemical_formula_sum            'C50 H53 N4 O2 P W2'
_chemical_formula_weight         1140.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.380(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1453(3)
_cell_length_b                   31.5276(12)
_cell_length_c                   15.2744(5)
_cell_measurement_reflns_used    11279
_cell_measurement_temperature    158(5)
_cell_measurement_theta_max      69.2620
_cell_measurement_theta_min      3.2180
_cell_measurement_wavelength     1.54184
_cell_volume                     4884.2(3)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      158(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.98
_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  0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.98
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23931
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.98
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.609
_diffrn_reflns_theta_min         2.803
_exptl_absorpt_coefficient_mu    9.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63222
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         3.498
_refine_diff_density_min         -2.591
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     536
_refine_ls_number_reflns         9027
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+216.7228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2338
_refine_ls_wR_factor_ref         0.2365
_reflns_number_gt                7857
_reflns_number_total             9027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00466_si_002.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4086095--4086096.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4086096
_platon_squeeze_void_probe_radius 1.20