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_7042473
_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_compound_source        'dichloromethane/petroleum ether'
_chemical_formula_moiety         'C36 H54 Mo2 O2 P2 S2, 2(C32 H12 B F24)'
_chemical_formula_sum            'C100 H78 B2 F48 Mo2 O2 P2 S2'
_chemical_formula_weight         2563.18
_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
;
2016-11-21 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                82.240(2)
_cell_angle_beta                 79.614(4)
_cell_angle_gamma                79.716(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0227(6)
_cell_length_b                   14.4107(3)
_cell_length_c                   28.5960(10)
_cell_measurement_reflns_used    15384
_cell_measurement_temperature    152(4)
_cell_measurement_theta_max      69.7670
_cell_measurement_theta_min      3.3540
_cell_volume                     5560.9(3)
_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_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      152(4)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47347
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.829
_diffrn_reflns_theta_min         3.160
_exptl_absorpt_coefficient_mu    3.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2564
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.134
_refine_diff_density_min         -2.868
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1581
_refine_ls_number_reflns         20596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0849
_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^)+(0.1350P)^2^+15.5302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14140
_reflns_number_total             20596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00132k2.cif
_cod_data_source_block           compound9
_cod_database_code               7042473
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.532
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              73384
_shelx_fab_checksum              99625