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_7708034
_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         'C19 H11 O10 P Se W2'
_chemical_formula_sum            'C19 H11 O10 P Se W2'
_chemical_formula_weight         876.90
_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                66.5430(10)
_cell_angle_beta                 78.3160(10)
_cell_angle_gamma                72.3750(10)
_cell_formula_units_Z            4
_cell_length_a                   9.61900(10)
_cell_length_b                   15.3701(2)
_cell_length_c                   18.5803(3)
_cell_measurement_reflns_used    22720
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.3910
_cell_measurement_theta_min      4.7990
_cell_volume                     2391.11(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.76a (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_environment      N~2~
_diffrn_ambient_temperature      123.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2715
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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     12.00 101.00   0.50    1.00    --   41.19  57.00  30.00  178
  2  \w    -13.00  64.00   0.50    1.00    --   41.19 -38.00  60.00  154
  3  \w    -28.00  74.00   0.50    1.00    --   41.19 -77.00-120.00  204
  4  \w     29.00  67.00   0.50    2.00    --   93.50 -93.00 132.86   76
  5  \w     73.00 123.00   0.50    2.00    --   93.50 -93.00 -33.11  100
  6  \w     10.00  49.00   0.50    2.00    --   93.50 -15.00-150.00   78
  7  \w     12.00  39.00   0.50    2.00    --   93.50 -93.00 -33.11   54
  8  \w     23.00 120.00   0.50    2.00    --   93.50 -77.00-120.00  194
  9  \w     75.00 164.00   0.50    2.00    --   93.50  30.00-150.00  178
 10  \w     19.00  56.00   0.50    2.00    --   93.50 -61.00 -30.00   74
 11  \w     77.00 124.00   0.50    2.00    --   93.50 -61.00 -30.00   94
 12  \w     52.00  77.00   0.50    2.00    --   93.50 -45.00 -90.00   50
 13  \w     73.00 105.00   0.50    2.00    --   93.50 125.00 -30.00   64
 14  \w     85.00 111.00   0.50    2.00    --   93.50 -15.00-150.00   52
 15  \w     44.00  75.00   0.50    2.00    --   93.50-125.00 150.00   62
 16  \w    117.00 143.00   0.50    2.00    --   93.50 -15.00-150.00   52
 17  \w     37.00  68.00   0.50    2.00    --   93.50 -30.00 -60.00   62
 18  \w     83.00 131.00   0.50    2.00    --   93.50 -93.00 132.86   96
 19  \w     17.00  53.00   0.50    2.00    --   93.50 -77.00  60.00   72
 20  \w     66.00 120.00   0.50    2.00    --   93.50 -77.00  60.00  108
 21  \w     22.00  78.00   0.50    2.00    --   93.50 -61.00 -90.00  112
 22  \w     94.00 123.00   0.50    2.00    --   93.50 -61.00 -90.00   58
 23  \w     20.00  47.00   0.50    2.00    --   93.50-125.00 -90.00   54
 24  \w     58.00  92.00   0.50    2.00    --   93.50-125.00 -90.00   68
 25  \w     54.00 172.00   0.50    2.00    --   93.50  15.00 150.00  236
 26  \w     20.00  77.00   0.50    2.00    --   93.50 -45.00 120.00  114
 27  \w     97.00 123.00   0.50    2.00    --   93.50 -93.00-179.62   52
 28  \w    123.00 164.00   0.50    2.00    --   93.50 125.00 -30.00   82
 29  \w     51.00  77.00   0.50    2.00    --   93.50 -93.00-179.62   52
 30  \w   -120.00  -8.00   0.50    1.00    --  -41.19 -77.00  90.00  224
 31  \w      8.00 120.00   0.50    1.00    --   41.19  77.00-150.00  224
 32  \w     -3.00  95.00   0.50    1.00    --   41.19-125.00   0.00  196
 33  \w     12.00 115.00   0.50    1.00    --   41.19  57.00 120.00  206
 34  \w     12.00 115.00   0.50    1.00    --   41.19  57.00 -30.00  206
 35  \w     63.00 163.00   0.50    2.00    --   93.50  61.00   0.00  200
 36  \w     66.00 168.00   0.50    2.00    --   93.50  45.00 -60.00  204
;
_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      0.0153893000
_diffrn_orient_matrix_UB_12      -0.1060207000
_diffrn_orient_matrix_UB_13      0.0588169000
_diffrn_orient_matrix_UB_21      -0.0257199000
_diffrn_orient_matrix_UB_22      0.0361711000
_diffrn_orient_matrix_UB_23      0.0690690000
_diffrn_orient_matrix_UB_31      -0.1661083000
_diffrn_orient_matrix_UB_32      0.0129158000
_diffrn_orient_matrix_UB_33      0.0034044000
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29701
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         3.235
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.365
_exptl_absorpt_correction_T_max  0.116
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.76a (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            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.436
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.330
_refine_diff_density_min         -2.630
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0.00082(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         8372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0494P)^2^+0.1860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8226
_reflns_number_total             8372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01866c2.cif
_cod_data_source_block           gl13_ap_abs_ana
_cod_depositor_comments
;
Adding full bibliography for 7708032--7708039.cif.

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H22 O20 P2 Se2 W4'
_cod_original_formula_weight         1753.81
_cod_original_formula_moiety         '2(C19 H11 O10 P Se W2)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2391.12(6)
_cod_database_code               7708034
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H22O20P2Se2W4
_shelx_estimated_absorpt_t_max   0.070
_shelx_estimated_absorpt_t_min   0.029
_reflns_odcompleteness_completeness 97.90
_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:
 C32(H32), C15(H15), C34(H34), C13(H13)
2.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              13945
_shelx_hkl_checksum              40173
_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 3.491
_oxdiff_exptl_absorpt_empirical_full_min 0.595