Cycloaddition Reactions of the Phosphinidene-Bridged Complex [Mo<sub>2</sub>Cp(μ-κ<sup>1</sup>:κ<sup>1</sup>,η<sup>5</sup>-PC<sub>5</sub>H<sub>4</sub>)(CO)<sub>2</sub>(η<sup>6</sup>-HMes*)] with Diazoalkanes and Other Heterocumulenes.
Albuerne, Isabel G.; Alvarez, M. Angeles; Amor, Inmaculada; García, M Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Inorganic chemistry 55 (2016) 10680–10691; doi:10.1021/acs.inorgchem.6b01930

data_4349127
_publ_section_title
;
 Cycloaddition Reactions of the Phosphinidene-Bridged Complex
 [Mo<sub>2</sub>Cp(\m-\k<sup>1</sup>:\k<sup>1</sup>,\h<sup>5</sup>-PC<sub>5</sub>H<sub>4</sub>)(CO)<sub>2</sub>(\h<sup>6</sup>-HMes*)]
 with Diazoalkanes and Other Heterocumulenes.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10680
_journal_page_last               10691
_journal_paper_doi               10.1021/acs.inorgchem.6b01930
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C37 H44 Mo2 N O2 P S'
_chemical_formula_sum            'C37 H44 Mo2 N O2 P S'
_chemical_formula_weight         789.64
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.834(5)
_cell_angle_beta                 106.289(5)
_cell_angle_gamma                95.765(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5874(6)
_cell_length_b                   11.1625(7)
_cell_length_c                   15.7439(9)
_cell_measurement_reflns_used    9449
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      69.6940
_cell_measurement_theta_min      4.3800
_cell_measurement_wavelength     1.54184
_cell_volume                     1760.43(19)
_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      153(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_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  0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15400
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.683
_diffrn_reflns_theta_min         2.952
_exptl_absorpt_coefficient_mu    7.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.719
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.6192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                5914
_reflns_number_total             6488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01930_si_002.cif
_cod_data_source_block           compound3
_cod_database_code               4349127
_oxdiff_exptl_absorpt_empirical_full_min 0.583
_oxdiff_exptl_absorpt_empirical_full_max 2.527
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;