One-step synthesis and P-H bond cleavage reactions of the phosphanyl complex syn-[MoCp{PH(2,4,6-C<sub>6</sub>H<sub>2</sub><sup>t</sup>Bu<sub>3</sub>)}(CO)<sub>2</sub>] to give heterometallic phosphinidene-bridged derivatives.
Alvarez, M. Angeles; Burgos, Mónica; García, M Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Vega, Patricia; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14585–14589; doi:10.1039/c9dt02382h

data_7701172
_publ_section_title
;
 One-step synthesis and P-H bond cleavage reactions of the phosphanyl
 complex
 syn-[MoCp{PH(2,4,6-C<sub>6</sub>H<sub>2</sub><sup>t</sup>Bu<sub>3</sub>)}(CO)<sub>2</sub>]
 to give heterometallic phosphinidene-bridged derivatives.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14585
_journal_page_last               14589
_journal_paper_doi               10.1039/c9dt02382h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H34 Mo O7 P Re'
_chemical_formula_sum            'C30 H34 Mo O7 P Re'
_chemical_formula_weight         819.69
_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   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-04-08 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                74.056(3)
_cell_angle_beta                 81.568(3)
_cell_angle_gamma                82.695(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3435(3)
_cell_length_b                   10.6128(3)
_cell_length_c                   14.9254(4)
_cell_measurement_reflns_used    10009
_cell_measurement_temperature    149.8(2)
_cell_measurement_theta_max      69.3610
_cell_measurement_theta_min      4.3350
_cell_volume                     1551.84(8)
_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      149.8(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.958
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13329
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.503
_diffrn_reflns_theta_min         4.339
_exptl_absorpt_coefficient_mu    11.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense green'
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             804
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane /petroleum ether'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5125
_reflns_number_total             5583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02382h3.cif
_cod_data_source_block           compound2
_cod_depositor_comments          'Adding full bibliography for 7701172.cif.'
_cod_database_code               7701172
_shelx_shelxl_version_number     2016/6
_oxdiff_exptl_absorpt_empirical_full_min 0.469
_oxdiff_exptl_absorpt_empirical_full_max 3.733
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              95912