Reactions of the unsaturated methyl-bridged complexes [Mo2Cp2(μ-CH3)(μ-P Bu2)(CO)x] (x = 1, 2) towards transition metal carbonyls: convenient dehydrogenative route to heterometallic methylidyne-bridged clusters
Alvarez, M. Angeles; Casado-Ruano, Melodie; García, M. Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Journal of Organometallic Chemistry 959 (2022) 122206–; doi:10.1016/j.jorganchem.2021.122206

data_4038973
_publ_section_title
;
 Reactions of the unsaturated methyl-bridged complexes
 [Mo2Cp2(\m-CH3)(\m-P Bu2)(CO)x] (x&#x00A0;=&#x00A0;1, 2) towards
 transition metal carbonyls: convenient dehydrogenative route to
 heterometallic methylidyne-bridged clusters
;
_journal_name_full               'Journal of Organometallic Chemistry'
_journal_page_first              122206
_journal_paper_doi               10.1016/j.jorganchem.2021.122206
_journal_volume                  959
_journal_year                    2022
_chemical_formula_moiety         'C25 H31 Fe Mo2 O6 P'
_chemical_formula_sum            'C25 H31 Fe Mo2 O6 P'
_chemical_formula_weight         706.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 113.905(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3932(3)
_cell_length_b                   17.6468(2)
_cell_length_c                   18.7329(4)
_cell_measurement_reflns_used    13558
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      69.4910
_cell_measurement_theta_min      2.9210
_cell_volume                     5256.55(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      150.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.666
_diffrn_reflns_theta_min         2.927
_exptl_absorpt_coefficient_mu    12.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45024
_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            brown
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.569
_refine_diff_density_min         -1.437
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0420P)^2^+10.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8528
_reflns_number_total             9760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JOC-2022-959-122206.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        5256.55(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4038973
_oxdiff_exptl_absorpt_empirical_full_min 0.643
_oxdiff_exptl_absorpt_empirical_full_max 1.937
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              86165
_shelx_hkl_checksum              68122