Development of sterically hindered siloxide-functionalized polyoxotungstates for the complexation of 5d-metals.
Auvray, Thomas; Nachtigall, Olaf; Brennessel, William W.; Jones, William D.; Matson, Ellen M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4300–4310; doi:10.1039/d1dt00256b

data_7706755
_publ_section_title
;
 Development of sterically hindered siloxide-functionalized
 polyoxotungstates for the complexation of 5d-metals.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4300
_journal_page_last               4310
_journal_paper_doi               10.1039/d1dt00256b
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C30 H24 D16 Hf O40 P Si3 W9, 3(C24 H52 N), 0.84(C4 D8 O)'
_chemical_formula_sum            'C105.39 H180 D22.77 Hf N3 O40.85 P Si3 W9'
_chemical_formula_weight         4136.93
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-14
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-01-25 deposited with the CCDC.	2021-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6019(2)
_cell_length_b                   19.8230(2)
_cell_length_c                   29.5100(2)
_cell_measurement_reflns_used    50074
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3530
_cell_measurement_theta_min      2.6840
_cell_volume                     13734.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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     86.00 154.00   0.50    5.17    --  105.75  77.00   0.00  136
  2  \w    104.00 178.00   0.50    5.17    --  105.75  52.00 103.00  148
  3  \w    104.00 154.00   0.50    5.17    --  105.75  30.00  90.00  100
  4  \w     63.00 103.00   0.50    1.29    --   49.75  52.00 103.00   80
  5  \w    102.00 177.00   0.50    5.17    --  105.75  30.00  30.00  150
  6  \w    105.00 154.00   0.50    5.17    --  105.75  30.00-180.00   98
  7  \w    -56.00 -31.00   0.50    5.17    --  -84.25  52.00 103.00   50
  8  \w    -51.00 -26.00   0.50    1.29    --  -49.75  52.00 103.00   50
  9  \w    -22.00  22.00   0.50    1.29    --  -49.75  52.00 103.00   88
 10  \w    -37.00 -12.00   0.50    5.17    --  -84.25  45.00  30.00   50
 11  \w    -38.00 -13.00   0.50    5.17    --  -84.25  45.00 -90.00   50
 12  \w     -2.00  23.00   0.50    1.29    --  -49.75  19.00-120.00   50
 13  \w     -4.00  24.00   0.50    1.29    --  -49.75  19.00 -90.00   56
 14  \w    -23.00   9.00   0.50    1.29    --   49.75 -19.00 -30.00   64
 15  \w     35.00  61.00   0.50    5.17    --  105.75 -61.00 150.00   52
 16  \w     50.00  80.00   0.50    5.17    --  105.75 -61.00  90.00   60
 17  \w     36.00  75.00   0.50    5.17    --  105.75 -61.00  30.00   78
 18  \w     36.00  69.00   0.50    5.17    --  105.75 -77.00  30.00   66
 19  \w     45.00  80.00   0.50    5.17    --  105.75 -61.00  60.00   70
 20  \w     34.00  79.00   0.50    5.17    --  105.75 -61.00 120.00   90
 21  \w     83.00 127.00   0.50    5.17    --  105.75 -77.00  30.00   88
 22  \w      3.00  30.00   0.50    1.29    --   49.75 -52.00 -42.00   54
 23  \w     36.00  75.00   0.50    5.17    --  105.75 -61.00 -90.00   78
 24  \w     51.00  78.00   0.50    5.17    --  105.75 -61.00 -60.00   54
 25  \w     34.00  64.00   0.50    5.17    --  105.75 -52.00 -42.00   60
 26  \w     84.00 109.00   0.50    5.17    --  105.75 -94.00 -30.00   50
 27  \w     69.00 106.00   0.50    5.17    --  105.75 -94.00 -90.00   74
 28  \w     44.00 116.00   0.50    5.17    --  105.75-125.00 -90.00  144
 29  \w     41.00 104.00   0.50    5.17    --  105.75 -94.00-120.00  126
 30  \w     37.00  62.00   0.50    5.17    --  105.75-125.00-180.00   50
 31  \w     89.00 115.00   0.50    5.17    --  105.75-125.00-180.00   52
 32  \w     41.00  67.00   0.50    5.17    --  105.75 -94.00 -90.00   52
 33  \w     41.00  68.00   0.50    5.17    --  105.75 -94.00 -30.00   54
 34  \w   -121.00 -39.00   0.50    1.29    --  -49.75 -52.00 -42.00  164
 35  \w   -139.00-114.00   0.50    5.17    --  -84.25 -52.00 -42.00   50
 36  \w   -116.00 -80.00   0.50    1.29    --  -49.75-125.00 -90.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0224600000
_diffrn_orient_matrix_UB_12      -0.0425647000
_diffrn_orient_matrix_UB_13      -0.0416996000
_diffrn_orient_matrix_UB_21      -0.0495728000
_diffrn_orient_matrix_UB_22      -0.0250355000
_diffrn_orient_matrix_UB_23      0.0257345000
_diffrn_orient_matrix_UB_31      -0.0366502000
_diffrn_orient_matrix_UB_32      0.0599795000
_diffrn_orient_matrix_UB_33      -0.0188344000
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            142062
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.924
_diffrn_reflns_theta_min         2.690
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_description       block
_exptl_crystal_F_000             7911
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.105
_refine_diff_density_min         -2.694
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1566
_refine_ls_number_reflns         28793
_refine_ls_number_restraints     373
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0754P)^2^+64.4201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24803
_reflns_number_total             28793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00256b2.cif
_cod_data_source_block           jonon34
_cod_depositor_comments
'Adding full bibliography for 7706755--7706757.cif.'
_cod_database_code               7706755
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.372
_diffrn_oxdiff_digest_frames
;
015b5b46eb80dec18d31f9973dd00358c202808ef53
;
_diffrn_oxdiff_digest_hkl
;
01e005b932f455c1417ef1145496993ff0d698
;
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O41-C103 = O41-C106
 1.44 with sigma of 0.02
 C103-C104 = C104-C105 = C105-C106
 1.53 with sigma of 0.02
 C24-C25 \\sim C24-C25' \\sim C25-C26 \\sim C25'-C26
 with sigma of 0.01
 N1-C49 \\sim N1-C49'
 with sigma of 0.01
 N3-C97 \\sim N3-C97'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C75 \\sim C76 \\sim C77 \\sim C78: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.01
C93 \\sim C94 \\sim C95 \\sim C96: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C25) = Uanis(C25')
Uanis(C97) = Uanis(C97')
Uanis(C98) = Uanis(C98')
Uanis(C99) = Uanis(C99')
Uanis(C100) = Uanis(C00')
Uanis(C101) = Uanis(C01')
Uanis(C102) = Uanis(C02')
4. Rigid body (RIGU) restrains
 C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49', C50', C51', C52', C53', C54'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O41, C103, C104, C105, C106
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C97, C98, C99, C100, C101, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C49, C50, C51, C52, C53, C54} sigma for 1-2: 0.02, 1-3: 0.04
as
{C49', C50', C51', C52', C53', C54'}
{N3, C85, C86, C87, C88, C89, C90} sigma for 1-2: 0.02, 1-3: 0.04
{N3, C91, C92, C93, C94, C95, C96} sigma for 1-2: 0.02, 1-3: 0.04
{N3, C97, C98, C99, C100, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
{N3, C97', C98', C99', C00', C01', C02'} sigma for 1-2: 0.02, 1-3: 0.04
as
{N3, C79, C80, C81, C82, C83, C84}
{C97, C98, C99, C100, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as
{C97', C98', C99', C00', C01', C02'}
{O41, C106, C105, C104, C103} sigma for 1-2: 0.02, 1-3: 0.04
as
{O41, C103, C104, C105, C106}
6. Others
 Sof(D24C)=Sof(D24D)=Sof(C25')=Sof(D25C)=Sof(D25D)=Sof(D26C)=Sof(D26D)=1-FVAR(1)
 Sof(D24A)=Sof(D24B)=Sof(C25)=Sof(D25A)=Sof(D25B)=Sof(D26A)=Sof(D26B)=FVAR(1)
 Sof(C49')=Sof(H49C)=Sof(H49D)=Sof(C50')=Sof(H50C)=Sof(H50D)=Sof(C51')=
 Sof(H51C)=Sof(H51D)=Sof(C52')=Sof(H52C)=Sof(H52D)=Sof(C53')=Sof(H53C)=
 Sof(H53D)=Sof(C54')=Sof(H54D)=Sof(H54E)=Sof(H54F)=1-FVAR(2)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=
 Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(C97')=Sof(H97C)=Sof(H97D)=Sof(C98')=Sof(H98C)=Sof(H98D)=Sof(C99')=
 Sof(H99C)=Sof(H99D)=Sof(C00')=Sof(H00A)=Sof(H00B)=Sof(C01')=Sof(H01A)=
 Sof(H01B)=Sof(C02')=Sof(H02A)=Sof(H02B)=Sof(H02C)=1-FVAR(3)
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=
 Sof(H99B)=Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(C101)=Sof(H10C)=Sof(H10D)=
 Sof(C102)=Sof(H10E)=Sof(H10F)=Sof(H10G)=FVAR(3)
 Sof(O41)=Sof(C103)=Sof(D10A)=Sof(D10B)=Sof(C104)=Sof(D10C)=Sof(D10D)=
 Sof(C105)=Sof(D10E)=Sof(D10F)=Sof(C106)=Sof(D10G)=Sof(D10H)=FVAR(4)
7.a Secondary CH2 refined with riding coordinates:
 C23(D23A,D23B), C24(D24A,D24B), C24(D24C,D24D), C25(D25A,D25B), C25'(D25C,
 D25D), C26(D26A,D26B), C26(D26C,D26D), C27(D27A,D27B), C28(D28A,D28B),
 C29(D29A,D29B), C30(D30A,D30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
  C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C49'(H49C,H49D), C50'(H50C,
 H50D), C51'(H51C,H51D), C52'(H52C,H52D), C53'(H53C,H53D), C55(H55A,H55B),
 C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C61(H61A,H61B),
  C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
  C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
 C89(H89A,H89B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B),
  C95(H95A,H95B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,
 H10B), C101(H10C,H10D), C97'(H97C,H97D), C98'(H98C,H98D), C99'(H99C,H99D),
 C00'(H00A,H00B), C01'(H01A,H01B), C103(D10A,D10B), C104(D10C,D10D), C105(D10E,
 D10F), C106(D10G,D10H)
7.b Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C54'(H54D,H54E,H54F), C78(H78A,H78B,H78C), C84(H84A,H84B,
 H84C), C96(H96A,H96B,H96C), C102(H10E,H10F,H10G), C02'(H02A,H02B,H02C)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
7.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C36(H36A,H36B,
 H36C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C60(H60A,H60B,H60C), C66(H66A,
 H66B,H66C), C72(H72A,H72B,H72C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              16387
_shelx_hkl_checksum              68653
_olex2_submission_original_sample_id jonon34
_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 1.926
_oxdiff_exptl_absorpt_empirical_full_min 0.536