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_7708035
_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         'C20 H10 O8 Se2 W2'
_chemical_formula_sum            'C20 H10 O8 Se2 W2'
_chemical_formula_weight         903.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 102.976(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3332(5)
_cell_length_b                   7.2060(2)
_cell_length_c                   17.1601(5)
_cell_measurement_reflns_used    1885
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      71.2320
_cell_measurement_theta_min      4.9500
_cell_volume                     2209.11(11)
_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 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.928
_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     90.00 115.00   0.50   10.00    --   41.44  57.00 -90.00   50
  2  \w     69.00 101.00   0.50   10.00    --   41.44 135.00 175.00   64
  3  \w     27.00 116.00   0.50   10.00    --   41.44  38.00-180.00  178
  4  \w     18.00  77.00   0.50   10.00    --   41.44  57.00 -90.00  118
  5  \w     61.00  92.00   0.50   35.00    --  108.74-135.00 -70.00   62
  6  \w     79.00 178.00   0.50   35.00    --  108.74  30.00-180.00  198
  7  \w     38.00  65.00   0.50   35.00    --  108.74 -30.00 150.00   54
  8  \w     32.00  69.00   0.50   35.00    --  108.74 -30.00   0.00   74
  9  \w     82.00 168.00   0.50   35.00    --  108.74  30.00 -90.00  172
 10  \w     37.00  91.00   0.50   35.00    --  108.74-125.00 -30.00  108
 11  \w    -99.00 -18.00   0.50   10.00    --  -41.44 125.00 120.00  162
 12  \w    -34.00  59.00   0.50   10.00    --   41.44 -38.00-120.00  186
 13  \w     12.00  26.00   0.50   10.00    --   41.44  57.00  30.00   28
;
_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      0.0684138000
_diffrn_orient_matrix_UB_12      0.0595723000
_diffrn_orient_matrix_UB_13      0.0650163000
_diffrn_orient_matrix_UB_21      -0.0525526000
_diffrn_orient_matrix_UB_22      0.0778282000
_diffrn_orient_matrix_UB_23      0.0505297000
_diffrn_orient_matrix_UB_31      -0.0001317000
_diffrn_orient_matrix_UB_32      -0.1901278000
_diffrn_orient_matrix_UB_33      0.0411566000
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4009
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.958
_diffrn_reflns_theta_min         4.951
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.147
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.126
_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    2.718
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0605P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1852
_reflns_number_total             2077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           gl7_2_lena
_cod_depositor_comments
'Adding full bibliography for 7708032--7708039.cif.'
_cod_database_code               7708035
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H10 Se2 W2 O8'
_reflns_odcompleteness_completeness 96.46
_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:
 C5(H5), C2(H2), C4(H4), C6(H6), C3(H3)
;
_shelx_res_checksum              74725
_shelx_hkl_checksum              58082
_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 1.327
_oxdiff_exptl_absorpt_empirical_full_min 0.718