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_7708033
_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 As O10 S W2'
_chemical_formula_sum            'C16 H5 As O10 S W2'
_chemical_formula_weight         831.88
_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'
_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                90
_cell_angle_beta                 99.533(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.97820(10)
_cell_length_b                   16.3547(2)
_cell_length_c                   18.6493(3)
_cell_measurement_reflns_used    10417
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.5740
_cell_measurement_theta_min      4.7890
_cell_volume                     2098.98(5)
_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      123.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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    -93.00 -27.00   0.50    4.00    --  -41.53 125.00 -30.00  132
  2  \w    -34.00  66.00   0.50    4.00    --   41.53 -38.00-150.00  200
  3  \w     82.00 134.00   0.50   17.50    --   93.50 178.00 -30.00  104
  4  \w     37.00  63.00   0.50   17.50    --   93.50 178.00 -30.00   52
  5  \w     67.00 117.00   0.50   17.50    --   93.50  15.00 -30.00  100
  6  \w     25.00  51.00   0.50   17.50    --   93.50 -93.00 157.32   52
  7  \w     11.00  83.00   0.50   17.50    --   93.50 -95.00 120.00  144
  8  \w     58.00 132.00   0.50   17.50    --   93.50 -93.00 157.32  148
  9  \w     76.00 166.00   0.50   17.50    --   93.50  30.00-150.00  180
 10  \w     18.00  80.00   0.50   17.50    --   93.50 -95.00   0.00  124
 11  \w     44.00  75.00   0.50   17.50    --   93.50 -45.00-120.00   62
 12  \w    143.00 171.00   0.50   17.50    --   93.50  15.00 -30.00   56
 13  \w     24.00  74.00   0.50   17.50    --   93.50 -45.00  90.00  100
 14  \w   -120.00  -8.00   0.50    4.00    --  -41.53 -77.00   0.00  224
 15  \w     12.00 115.00   0.50    4.00    --   41.53  57.00 150.00  206
 16  \w     12.00 115.00   0.50    4.00    --   41.53  57.00 -90.00  206
 17  \w     60.00 107.00   0.50   17.50    --   93.50  77.00 -30.00   94
 18  \w     63.00 168.00   0.50   17.50    --   93.50  61.00 120.00  210
 19  \w     66.00 168.00   0.50   17.50    --   93.50  45.00  60.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1332508000
_diffrn_orient_matrix_UB_12      -0.0705048000
_diffrn_orient_matrix_UB_13      0.0323478000
_diffrn_orient_matrix_UB_21      0.0533450000
_diffrn_orient_matrix_UB_22      0.0480976000
_diffrn_orient_matrix_UB_23      0.0715413000
_diffrn_orient_matrix_UB_31      -0.1716823000
_diffrn_orient_matrix_UB_32      -0.0398170000
_diffrn_orient_matrix_UB_33      0.0292997000
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16040
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.816
_diffrn_reflns_theta_max         66.815
_diffrn_reflns_theta_min         3.617
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.124
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.198
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.632
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+0.7859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3472
_reflns_number_total             3697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           gl61_lena
_cod_depositor_comments
'Adding full bibliography for 7708032--7708039.cif.'
_cod_database_code               7708033
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H5O10As1S1W2
_reflns_odcompleteness_completeness 98.49
_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:
 C6(H6), C2(H2), C5(H5), C3(H3), C4(H4)
;
_shelx_res_checksum              29558
_shelx_hkl_checksum              40995
_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 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.743