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_7708037
_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         'C23 H22 O5 Te2 W'
_chemical_formula_sum            'C23 H22 O5 Te2 W'
_chemical_formula_weight         817.45
_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                 145.249(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5396(12)
_cell_length_b                   18.5800(3)
_cell_length_c                   28.924(2)
_cell_measurement_reflns_used    12142
_cell_measurement_temperature    123
_cell_measurement_theta_max      72.5460
_cell_measurement_theta_min      3.7600
_cell_volume                     5067(2)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.972
_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    -37.00  69.00   2.00   25.00    --   40.72 -38.00-120.00   53
  2  \w     10.00 116.00   2.00   25.00    --   40.72  57.00  30.00   53
  3  \w     30.00  76.00   2.00   75.00    --  106.96 -45.00 -30.00   23
  4  \w     27.00  69.00   2.00   75.00    --  106.96 -30.00  90.00   21
  5  \w     20.00 146.00   2.00   75.00    --  106.96 -89.00 -63.48   63
  6  \w     27.00  69.00   2.00   75.00    --  106.96 -30.00 120.00   21
  7  \w     30.00  76.00   2.00   75.00    --  106.96 -45.00 150.00   23
  8  \w     78.00 178.00   2.00   75.00    --  106.96  45.00  60.00   50
  9  \w     25.00 141.00   2.00   75.00    --  106.96 -77.00 -30.00   58
 10  \w     27.00  69.00   2.00   75.00    --  106.96 -30.00-180.00   21
 11  \w      6.00 122.00   2.00   25.00    --   40.72  77.00 150.00   58
 12  \w     10.00 116.00   2.00   25.00    --   40.72  57.00 -90.00   53
 13  \w     30.00  92.00   2.00   75.00    --  106.96  15.00 -90.00   31
;
_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      0.0328988000
_diffrn_orient_matrix_UB_12      -0.0812393000
_diffrn_orient_matrix_UB_13      0.0153089000
_diffrn_orient_matrix_UB_21      0.0298866000
_diffrn_orient_matrix_UB_22      0.0033302000
_diffrn_orient_matrix_UB_23      -0.0382482000
_diffrn_orient_matrix_UB_31      0.1573019000
_diffrn_orient_matrix_UB_32      0.0163222000
_diffrn_orient_matrix_UB_33      0.0838637000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27607
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.941
_diffrn_reflns_theta_min         3.584
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.511
_exptl_absorpt_correction_T_max  0.460
_exptl_absorpt_correction_T_min  0.047
_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            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0423P)^2^+3.9184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9047
_reflns_number_total             9821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           lr53hex_abs2
_cod_depositor_comments
'Adding full bibliography for 7708032--7708039.cif.'
_cod_original_cell_volume        5066.6(13)
_cod_database_code               7708037
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35 H46 O5 Te2 W'
_shelx_estimated_absorpt_t_max   0.357
_shelx_estimated_absorpt_t_min   0.044
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C17(H17), C19(H19), C40(H40), C10(H10), C42(H42), C31(H31), C33(H33)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C37(H37A,H37B,H37C), C14(H14A,H14B,
 H14C), C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C13(H13A,
 H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C45(H45A,H45B,H45C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              57435
_shelx_hkl_checksum              94081
_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 2.909
_oxdiff_exptl_absorpt_empirical_full_min 0.609