Terminal vs. bridging coordination of CO and NO ligands after decarbonylation of [W2Cp2(μ-PR2)(CO)3(NO)] complexes (R = Ph, Cy). An experimental and computational study
Alvarez, M. Angeles; García, M. Esther; García-Vivó, Daniel; Rueda, M. Teresa; Ruiz, Miguel A.; Toyos, Adrián; Vega, M. Fernanda; Dalton Trans.  (2017) –; doi:10.1039/C7DT02243C

data_7043851
_publ_section_title
;
 Terminal vs. bridging coordination of CO and NO ligands after
 decarbonylation of [W2Cp2(\m-PR2)(CO)3(NO)] complexes (R = Ph, Cy). An
 experimental and computational study
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02243C
_journal_year                    2017
_chemical_formula_moiety         'C27 H41 N O6 P2 W2'
_chemical_formula_sum            'C27 H41 N O6 P2 W2'
_chemical_formula_weight         905.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-05-04 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.514(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0125(3)
_cell_length_b                   15.8531(5)
_cell_length_c                   18.6734(6)
_cell_measurement_reflns_used    8165
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.1663
_cell_measurement_theta_min      3.6572
_cell_volume                     3549.39(18)
_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      100.00(10)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.978
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15594
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.291
_diffrn_reflns_theta_min         3.660
_exptl_absorpt_coefficient_mu    12.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and petroleum ether'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+66.1530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5907
_reflns_number_total             6502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02243c3.cif
_cod_data_source_block           compound4b
_cod_database_code               7043851
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.324
_shelx_estimated_absorpt_t_max   0.499
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              40454
_shelx_fab_checksum              82273