Chemistry of CS2- and SCNPh-adducts of the pyramidal phosphinidene-bridged complex [Mo2Cp(μ-κ(1):κ(1),η(5)-PC5H4)(CO)2(η(6)-HMes*)(PMe3)].
Albuerne, Isabel G.; Alvarez, M. Angeles; García, M Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3510–3525; doi:10.1039/c7dt00132k

data_7042475
_publ_section_title
;
 Chemistry of CS2- and SCNPh-adducts of the pyramidal
 phosphinidene-bridged complex
 [Mo2Cp(\m-\k(1):\k(1),\h(5)-PC5H4)(CO)2(\h(6)-HMes*)(PMe3)].
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3510
_journal_page_last               3525
_journal_paper_doi               10.1039/c7dt00132k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C34 H48 Mo2 O2 P2 S2, 0.5(C6 H14)'
_chemical_formula_sum            'C37 H55 Mo2 O2 P2 S2'
_chemical_formula_weight         849.75
_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
;
2016-11-21 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5929(2)
_cell_length_b                   14.32660(10)
_cell_length_c                   18.1379(2)
_cell_measurement_reflns_used    8660
_cell_measurement_temperature    123.0(3)
_cell_measurement_theta_max      74.3538
_cell_measurement_theta_min      3.0820
_cell_volume                     4533.55(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      123.0(3)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17765
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.525
_diffrn_reflns_theta_min         3.945
_exptl_absorpt_coefficient_mu    6.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58405
_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            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/petroleum ether'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+1.3119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7633
_reflns_number_total             8899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00132k2.cif
_cod_data_source_block           compound2a
_cod_database_code               7042475
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.247
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              39845
_shelx_fab_checksum              78184