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_7042472
_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_absolute_configuration 'not determined'
_chemical_formula_moiety         'C32 H12 B F24, C41 H55 Cl Mo2 N O2 P2 S'
_chemical_formula_sum            'C73 H67 B Cl F24 Mo2 N O2 P2 S'
_chemical_formula_weight         1778.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.014(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4244(2)
_cell_length_b                   16.8423(3)
_cell_length_c                   16.8318(3)
_cell_measurement_reflns_used    10995
_cell_measurement_temperature    150.1(5)
_cell_measurement_theta_max      69.4440
_cell_measurement_theta_min      3.5240
_cell_volume                     3866.01(12)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.1(5)
_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_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21417
_diffrn_reflns_point_group_measured_fraction_full 0.771
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.610
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/petroleum ether'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 3073 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         10974
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+5.4008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.477
_reflns_Friedel_fraction_full    0.525
_reflns_Friedel_fraction_max     0.506
_reflns_number_gt                10169
_reflns_number_total             10974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00132k2.cif
_cod_data_source_block           compound8
_cod_database_code               7042472
_shelx_estimated_absorpt_t_min   0.353
_shelx_estimated_absorpt_t_max   0.840
_oxdiff_exptl_absorpt_empirical_full_min 0.685
_oxdiff_exptl_absorpt_empirical_full_max 2.030
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              47720