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_7708038
_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 Se W2'
_chemical_formula_sum            'C16 H5 O10 P Se W2'
_chemical_formula_weight         834.83
_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             2021-05-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.7400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.01510(10)
_cell_length_b                   16.4460(2)
_cell_length_c                   18.4907(2)
_cell_measurement_reflns_used    13435
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.7750
_cell_measurement_theta_min      4.8240
_cell_volume                     2102.53(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_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_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_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    -40.00  27.00   1.00    7.50    --   41.28 -19.00  90.00   67
  2  \w    -40.00  27.00   1.00    7.50    --   41.28 -19.00-180.00   67
  3  \w    -40.00  27.00   1.00    7.50    --   41.28 -19.00-150.00   67
  4  \w     30.00  71.00   1.00   22.50    --  104.28 -61.00-180.00   41
  5  \w     30.00  71.00   1.00   22.50    --  104.28 -61.00  30.00   41
  6  \w     30.00  71.00   1.00   22.50    --  104.28 -61.00-150.00   41
  7  \w     26.00  83.00   1.00   22.50    --  104.28-111.00 150.00   57
  8  \w     74.00 178.00   1.00   22.50    --  104.28  61.00 -90.00  104
  9  \w     30.00  71.00   1.00   22.50    --  104.28 -61.00 120.00   41
 10  \w     26.00 105.00   1.00   22.50    --  104.28 -77.00 -30.00   79
 11  \w     77.00 178.00   1.00   22.50    --  104.28  45.00  30.00  101
 12  \w     12.00 115.00   1.00    7.50    --   41.28  57.00 -30.00  103
 13  \w     -5.00 123.00   1.00    7.50    --   41.28  19.00-120.00  128
 14  \w     43.00 178.00   1.00   22.50    --  104.28  15.00-180.00  135
 15  \w     74.00 178.00   1.00   22.50    --  104.28  61.00 -30.00  104
 16  \w     74.00 178.00   1.00   22.50    --  104.28  61.00-150.00  104
 17  \w     74.00 178.00   1.00   22.50    --  104.28  61.00  60.00  104
 18  \w     26.00 105.00   1.00   22.50    --  104.28 -77.00-180.00   79
 19  \w     30.00  71.00   1.00   22.50    --  104.28 -61.00 -90.00   41
 20  \w    -99.00 -22.00   1.00    7.50    --  -41.28 125.00 -30.00   77
 21  \w     12.00 115.00   1.00    7.50    --   41.28  57.00  90.00  103
 22  \w     74.00 178.00   1.00   22.50    --  104.28  61.00 150.00  104
 23  \w     74.00 153.00   1.00   22.50    --  104.28  61.00-120.00   79
;
_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      -0.0410140000
_diffrn_orient_matrix_UB_12      -0.0506953000
_diffrn_orient_matrix_UB_13      0.0657433000
_diffrn_orient_matrix_UB_21      -0.1501714000
_diffrn_orient_matrix_UB_22      -0.0503968000
_diffrn_orient_matrix_UB_23      -0.0517847000
_diffrn_orient_matrix_UB_31      0.1593912000
_diffrn_orient_matrix_UB_32      -0.0605321000
_diffrn_orient_matrix_UB_33      -0.0119453000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22285
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.061
_diffrn_reflns_theta_min         3.620
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.108
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.148
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.637
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.641
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0481P)^2^+1.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3880
_reflns_number_total             4109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           lr131_abs2
_cod_depositor_comments
'Adding full bibliography for 7708032--7708039.cif.'
_cod_database_code               7708038
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H5 Se P W2 O10'
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.140
_reflns_odcompleteness_completeness 99.92
_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:
 C12(H12), C16(H16), C15(H15), C13(H13), C14(H14)
;
_shelx_res_checksum              3509
_shelx_hkl_checksum              95055
_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 1.553
_oxdiff_exptl_absorpt_empirical_full_min 0.642