The ditungsten decacarbonyl dianion.
Ostrowski, Joseph P. A.; Atkinson, Benjamin E.; Doyle, Laurence R.; Wooles, Ashley J.; Kaltsoyannis, Nikolas; Liddle, Stephen T.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9330–9335; doi:10.1039/d0dt01921f

data_7704670
_publ_section_title
;
 The ditungsten decacarbonyl dianion.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9330
_journal_page_last               9335
_journal_paper_doi               10.1039/d0dt01921f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C10 O10 W2, 2(C20 H40 K O8)'
_chemical_formula_sum            'C54 H88 K2 O27 W2'
_chemical_formula_weight         1615.14
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-16 deposited with the CCDC.	2020-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                104.271(5)
_cell_angle_beta                 97.866(4)
_cell_angle_gamma                96.771(3)
_cell_formula_units_Z            1
_cell_length_a                   10.3537(3)
_cell_length_b                   13.2809(7)
_cell_length_c                   13.4937(8)
_cell_measurement_reflns_used    7118
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4910
_cell_measurement_theta_min      3.1690
_cell_volume                     1758.93(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -46.00 -13.00   1.00    2.86    --   20.02 -57.00   0.00   33
  2  \w    -48.00  42.00   1.00    2.86    --   20.02 -57.00 -30.00   90
  3  \w    -20.00  25.00   1.00    2.86    --  -18.77 -99.00   0.00   45
  4  \w    -33.00  13.00   1.00    2.86    --  -18.77 -77.00  90.00   46
  5  \w    -53.00  45.00   1.00    2.86    --   20.02 -37.00  60.00   98
  6  \w    -34.00  -6.00   1.00    2.86    --  -18.77 -37.00-150.00   28
  7  \w    -24.00  47.00   1.00    2.86    --   20.02 -37.00-180.00   71
  8  \w     36.00  61.00   1.00    2.86    --   20.02-178.00 -30.00   25
  9  \w    -85.00   3.00   1.00    2.86    --  -18.77 -57.00-180.00   88
 10  \w     68.00  97.00   1.00    2.86    --   20.02 178.00  60.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0259322000
_diffrn_orient_matrix_UB_12      -0.0003691000
_diffrn_orient_matrix_UB_13      0.0513398000
_diffrn_orient_matrix_UB_21      0.0015977000
_diffrn_orient_matrix_UB_22      -0.0547156000
_diffrn_orient_matrix_UB_23      -0.0173134000
_diffrn_orient_matrix_UB_31      0.0650392000
_diffrn_orient_matrix_UB_32      0.0109840000
_diffrn_orient_matrix_UB_33      -0.0098217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6210
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.763
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.460
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.096
_refine_diff_density_max         3.414
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         6210
_refine_ls_number_restraints     1089
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0742P)^2^+12.1680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5398
_reflns_number_total             6210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01921f2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7704670.cif.'
_cod_original_cell_volume        1758.95(15)
_cod_database_code               7704670
_manchester_internal_diff_code   ASTL353
_manchester_internal_stl_name    THJO6
_manchester_internal_coll_client JO
_manchester_internal_coll_date   05/04/2018
_manchester_internal_process_date 10/04/2018
_manchester_internal_process_user AW
_manchester_internal_solution_date 10/04/2018
_manchester_internal_solution_user AW
_manchester_internal_refinement_date 16/09/2019
_manchester_internal_refinement_user AW
_manchester_internal_validation_date 16/09/2019
_manchester_internal_validation_user AW
_manchester_internal_archive_date 16/09/2019
_manchester_internal_archive_user AW
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H32  W O13 K'
_chemical_oxdiff_usercomment     JO
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.314
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(6)
 0.08(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3. Restrained distances
 O6-C6 = O6-C31 = O14-C30 = O7-C7 = O14-C29 = O7-C8 = O15-C28 = O8-C9 = O15-
 C27 = O8-C10 = O9-C32 = O9-C12 = O9-C35 = O9-C15 = O13-C22 = O13-C45 = O13-C25
 = O13-C42 = O11-C18 = O17-C36 = O17-C37 = O10-C17 = O10-C16 = O11-C19 = O12-
 C20 = O12-C21 = O19-C41 = O19-C40 = O18-C39 = O18-C38
 1.45 with sigma of 0.01
 C18-C17 = C38-C37 = C20-C19 = C40-C39 = C44-C43 = C25-C24 = C45-C44 = C43-C42
 = C23-C22 = C24-C23 = C34-C33 = C33-C32 = C14-C13 = C15-C14 = C35-C34 = C13-
 C12 = C27-C26 = C11-C10 = C9-C8 = C29-C28 = C31-C30 = C7-C6 = C21_$1-C16
 1.55 with sigma of 0.01
 K1-O6 \\sim K1-O7 \\sim K1-O8 \\sim K1-O15 \\sim K3-O19 \\sim K2-O12 \\sim
K2-O11 \\sim K3-O18 \\sim K2-O10 ~
 K3-O17
 with sigma of 0.01
 C23-C25 \\sim C22-C24 \\sim C44-C42 \\sim C43-C45 \\sim C35-C33 \\sim C32-C34
\\sim C12-C14 \\sim C15-C13
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O9 \\sim K1 \\sim O6 \\sim O15 \\sim O8 \\sim O7 \\sim O14 \\sim C12 \\sim C15
\\sim C32 \\sim C35 \\sim C6 \\sim C31 \\sim C27 \\sim C28 \\sim C9 \\sim C10
\\sim C7 \\sim C8 \\sim C29 \\sim C30 \\sim C13 \\sim C14 \\sim C33 \\sim C34
\\sim C26 \\sim C11 \\sim C18 \\sim K2 \\sim O13 \\sim O10 \\sim O12 \\sim O11
\\sim C25 \\sim K3 \\sim C22 \\sim C42 \\sim C45 \\sim C16 \\sim C17 \\sim C20
\\sim C21 \\sim C19 \\sim C24 \\sim O17 \\sim O18 \\sim O19 \\sim C23 \\sim C43
\\sim C44 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O9, K1, O6, O15, O8, O7, O14, C12, C15, C32, C35, C6, C31, C27, C28, C9, C10,
 C7, C8, C29, C30, C13, C14, C33, C34, C26, C11, C18, K2, O13, O10, O12, O11,
 C25, K3, C22, C42, C45, C16, C17, C20, C21, C19, C24, O17, O18, O19, C23, C43,
 C44, C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=1-FVAR(2)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(O14)=Sof(O15)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=1-FVAR(3)
 Sof(O7)=Sof(O8)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(3)
 Sof(O17)=Sof(O18)=Sof(O19)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=1-FVAR(4)
 Sof(K3)=0.5*(1-FVAR(5))
 Sof(K2)=0.5*FVAR(5)
 Sof(O10)=Sof(O11)=Sof(O12)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=
 Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B)
;
_shelx_res_checksum              34025
_shelx_fab_checksum              34239
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.725
_oxdiff_exptl_absorpt_empirical_full_min 0.785