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_4349129
_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         '2(C43 H49 Mo2 O2 P), C7 H8'
_chemical_formula_sum            'C93 H106 Mo4 O4 P2'
_chemical_formula_weight         1733.48
_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                103.176(4)
_cell_angle_beta                 91.152(4)
_cell_angle_gamma                109.283(5)
_cell_formula_units_Z            1
_cell_length_a                   9.5101(5)
_cell_length_b                   12.8133(7)
_cell_length_c                   17.9238(7)
_cell_measurement_reflns_used    10430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7175
_cell_measurement_theta_min      2.5386
_cell_measurement_wavelength     0.71073
_cell_volume                     1996.48(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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.933
_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  0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20633
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.818
_diffrn_reflns_theta_min         2.546
_exptl_absorpt_coefficient_mu    5.801
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.62081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+19.5848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1579
_reflns_number_gt                5704
_reflns_number_total             7536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01930_si_002.cif
_cod_data_source_block           compound5b
_cod_original_cell_volume        1996.47(18)
_cod_database_code               4349129