Reactivity of the pentelidene complexes [Cp*E{W(CO)<sub>5</sub>}<sub>2</sub>] (E = P, As) towards dichalcogenides and chalcogenols - synthesis of novel chalcogenopentelidene complexes.
Rummel, Lena; Lassandro, Giuliano; Seidl, Michael; Timoshkin, Alexey Y.; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12648–12654; doi:10.1039/d1dt01866c

data_7708032
_publ_section_title
;
 Reactivity of the pentelidene complexes
 [Cp*E{W(CO)<sub>5</sub>}<sub>2</sub>] (E = P, As) towards dichalcogenides
 and chalcogenols - synthesis of novel chalcogenopentelidene complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12648
_journal_page_last               12654
_journal_paper_doi               10.1039/d1dt01866c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C16 H5 O10 P S W2'
_chemical_formula_sum            'C16 H5 O10 P S W2'
_chemical_formula_weight         787.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                109.413(2)
_cell_angle_beta                 91.241(2)
_cell_angle_gamma                95.635(2)
_cell_formula_units_Z            4
_cell_length_a                   6.59340(10)
_cell_length_b                   17.2561(4)
_cell_length_c                   19.7432(4)
_cell_measurement_reflns_used    8754
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.4800
_cell_measurement_theta_min      4.1750
_cell_volume                     2104.83(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2715
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  71.00   0.50    3.00    --   41.19 -57.00  90.00  208
  2  \w     23.00 104.00   0.50    3.00    --   41.19  57.00-120.00  162
  3  \w     -3.00  95.00   0.50    3.00    --   41.19-125.00   0.00  196
  4  \w   -159.00-105.00   0.50   18.00    --  -83.00 -30.00-150.00  108
  5  \w     32.00  69.00   0.50   18.00    --  108.12 -30.00 -90.00   74
  6  \w     30.00  69.00   0.50   18.00    --  108.12 -30.00   0.00   78
  7  \w     92.00 130.00   0.50   18.00    --  108.12  45.00 -60.00   76
  8  \w     37.00  69.00   0.50   18.00    --  108.12 -30.00  60.00   64
  9  \w     30.00  64.00   0.50   18.00    --  108.12 -30.00-180.00   68
 10  \w     35.00  69.00   0.50   18.00    --  108.12 -30.00  30.00   68
 11  \w     25.00 144.00   0.50   18.00    --  108.12 -86.00-145.51  238
 12  \w     30.00  66.00   0.50   18.00    --  108.12 -30.00-150.00   72
 13  \w     84.00 177.00   0.50   18.00    --  108.12  30.00-180.00  186
 14  \w     45.00  75.00   0.50   18.00    --  108.12 -45.00 120.00   60
 15  \w     24.00 142.00   0.50   18.00    --  108.12 -89.00  24.95  236
 16  \w     12.00  84.00   0.50    3.00    --   41.19  57.00 150.00  144
 17  \w     12.00 115.00   0.50    3.00    --   41.19  57.00  60.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0155172000
_diffrn_orient_matrix_UB_12      0.0732078000
_diffrn_orient_matrix_UB_13      -0.0285191000
_diffrn_orient_matrix_UB_21      0.2219921000
_diffrn_orient_matrix_UB_22      -0.0141542000
_diffrn_orient_matrix_UB_23      -0.0188064000
_diffrn_orient_matrix_UB_31      -0.0760862000
_diffrn_orient_matrix_UB_32      -0.0592767000
_diffrn_orient_matrix_UB_33      -0.0755039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13300
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.827
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.032
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7270
_reflns_number_total             7859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           gl8c_lena
_cod_depositor_comments
'Adding full bibliography for 7708032--7708039.cif.'
_cod_database_code               7708032
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H5 O10 W2 P S'
_reflns_odcompleteness_completeness 96.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C16(H16), C31(H31), C30(H30), C32(H32), C12(H12),
 C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              22661
_shelx_hkl_checksum              35447
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.754