Reactive Coordinatively Saturated Mo(III) Complex: Exploiting the Adaptive Hapticity of Tris(tert-butoxy)silanolate Ligands
Pucino, Margherita; Allouche, Florian; Gordon, Christopher P.; Wörle, Michael; Mougel, Victor; Coperet, Christophe; Chemical Science  (2019) –; doi:10.1039/C9SC01955C

data_1551053
_publ_section_title
;
 Reactive Coordinatively Saturated Mo(III) Complex: Exploiting the
 Adaptive Hapticity of Tris(tert-butoxy)silanolate Ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01955C
_journal_year                    2019
_chemical_formula_moiety         'C36 H81 Mo O12 Si3'
_chemical_formula_sum            'C36 H81 Mo O12 Si3'
_chemical_formula_weight         886.21
_chemical_name_systematic        '[Mo(TBOS)3]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.521(4)
_cell_angle_beta                 95.866(4)
_cell_angle_gamma                93.602(3)
_cell_formula_units_Z            4
_cell_length_a                   14.2373(7)
_cell_length_b                   17.8493(7)
_cell_length_c                   19.9245(9)
_cell_measurement_reflns_used    5912
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.6647
_cell_measurement_theta_min      2.7821
_cell_volume                     4934.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -47.00   44.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6342   77.0000 -180.0000 91

  2 omega  -25.00   20.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6342  -99.0000  -30.0000 45

  3 omega  -65.00    0.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.6342  -57.0000   90.0000 65

  4 omega  -23.00   64.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1029  -99.0000  -60.0000 87

  5 omega  -25.00   64.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1029  -99.0000   90.0000 89

  6 omega    1.00   91.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1029   57.0000 -120.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0015702000
_diffrn_orient_matrix_UB_12      -0.0280231000
_diffrn_orient_matrix_UB_13      0.0210198000
_diffrn_orient_matrix_UB_21      0.0382536000
_diffrn_orient_matrix_UB_22      0.0208421000
_diffrn_orient_matrix_UB_23      0.0227602000
_diffrn_orient_matrix_UB_31      -0.0325570000
_diffrn_orient_matrix_UB_32      0.0206235000
_diffrn_orient_matrix_UB_33      0.0192097000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.2037
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43284
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.788
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.1884
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.1038
_refine_diff_density_max         1.377
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         19802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1606
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0613P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10565
_reflns_number_total             19802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           vm3985-8
_cod_database_code               1551053
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'Mo1 Si3 O12 C36 H81'
_reflns_odcompleteness_completeness 96.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H17A(0.08) H17B(0.08) H17C(0.08) H1A(0.064) H1B(0.064) H1C(0.064)
 H4A(0.063) H4B(0.063) H4C(0.063) H6A(0.086) H6B(0.086) H6C(0.086) H7A(0.06)
 H7B(0.06) H7C(0.06) H12G(0.055) H12H(0.055) H12I(0.055) H17D(0.071)
 H17E(0.071) H17F(0.071) H24A(0.061) H24B(0.061) H24C(0.061) H28A(0.058)
 H28B(0.058) H28C(0.058) H29A(0.063) H29B(0.063) H29C(0.063) H31A(0.061)
 H31B(0.061) H31C(0.061) H34A(0.066) H34B(0.066) H34C(0.066) H36A(0.076)
 H36B(0.076) H36C(0.076) H41A(0.071) H41B(0.071) H41C(0.071) H45A(0.085)
 H45B(0.085) H45C(0.085) H48A(0.092) H48B(0.092) H48C(0.092) H54A(0.057)
 H54B(0.057) H54C(0.057) H56A(0.057) H56B(0.057) H56C(0.057) H57A(0.067)
 H57B(0.067) H57C(0.067) H60A(0.079) H60B(0.079) H60C(0.079) H63A(0.066)
 H63B(0.066) H63C(0.066) H72A(0.059) H72B(0.059) H72C(0.059) H74A(0.053)
 H74B(0.053) H74C(0.053) H76A(0.065) H76B(0.065) H76C(0.065) H78A(0.064)
 H78B(0.064) H78C(0.064) H80A(0.109) H80B(0.109) H80C(0.109) H82A(0.072)
 H82B(0.072) H82C(0.072) H84A(0.08) H84B(0.08) H84C(0.08) H85A(0.059)
 H85B(0.059) H85C(0.059) H88A(0.062) H88B(0.062) H88C(0.062) H90A(0.085)
 H90B(0.085) H90C(0.085) H94A(0.074) H94B(0.074) H94C(0.074) H96A(0.07)
 H96B(0.07) H96C(0.07) H10A(0.057) H10B(0.057) H10C(0.057) H10D(0.059)
 H10E(0.059) H10F(0.059) H10G(0.06) H10H(0.06) H10I(0.06) H10J(0.076)
 H10K(0.076) H10L(0.076) H11D(0.062) H11E(0.062) H11F(0.062) H11G(0.081)
 H11H(0.081) H11I(0.081) H11A(0.075) H11B(0.075) H11C(0.075) H12J(0.064)
 H12K(0.064) H12L(0.064) H12M(0.08) H12N(0.08) H12O(0.08) H12A(0.059)
 H12B(0.059) H12C(0.059) H12D(0.067) H12E(0.067) H12F(0.067) H13A(0.075)
 H13B(0.075) H13C(0.075) H13G(0.078) H13H(0.078) H13I(0.078) H13J(0.073)
 H13K(0.073) H13L(0.073) H13D(0.093) H13E(0.093) H13F(0.093) H13M(0.071)
 H13N(0.071) H13O(0.071) H14A(0.074) H14B(0.074) H14C(0.074) H14D(0.077)
 H14E(0.077) H14F(0.077) H14J(0.094) H14K(0.094) H14L(0.094) H14G(0.106)
 H14H(0.106) H14I(0.106) H15A(0.075) H15B(0.075) H15C(0.075)
 Fixed X: H17A(0.353) H17B(0.2623) H17C(0.3594) H1A(-0.2012) H1B(-0.3046) H1C(-
 0.2778) H4A(-0.3822) H4B(-0.3937) H4C(-0.3822) H6A(-0.1389) H6B(-0.0971) H6C(-
 0.1488) H7A(0.1694) H7B(0.0808) H7C(0.1668) H12G(0.4163) H12H(0.4955)
 H12I(0.4789) H17D(0.432) H17E(0.4336) H17F(0.3617) H24A(-0.2398) H24B(-0.2564)
 H24C(-0.1575) H28A(0.2612) H28B(0.1736) H28C(0.2205) H29A(0.0022) H29B(-
 0.0142) H29C(0.0774) H31A(0.3383) H31B(0.3942) H31C(0.2843) H34A(-0.1674)
 H34B(-0.2425) H34C(-0.1418) H36A(0.6579) H36B(0.6454) H36C(0.5566)
 H41A(0.6471) H41B(0.6653) H41C(0.6909) H45A(-0.0407) H45B(-0.0119)
 H45C(0.0037) H48A(0.5263) H48B(0.6313) H48C(0.5646) H54A(-0.0753) H54B(-
 0.0537) H54C(-0.0169) H56A(0.6821) H56B(0.7502) H56C(0.7105) H57A(0.8036)
 H57B(0.8636) H57C(0.8561) H60A(0.1673) H60B(0.1019) H60C(0.057) H63A(0.4513)
 H63B(0.5024) H63C(0.4477) H72A(0.3041) H72B(0.3911) H72C(0.3069) H74A(0.2114)
 H74B(0.2406) H74C(0.2801) H76A(0.0487) H76B(-0.0338) H76C(-0.0113)
 H78A(0.2996) H78B(0.4071) H78C(0.3775) H80A(0.4962) H80B(0.4649) H80C(0.3925)
 H82A(0.3797) H82B(0.2902) H82C(0.3059) H84A(0.4825) H84B(0.5723) H84C(0.5401)
 H85A(0.2161) H85B(0.1756) H85C(0.1078) H88A(-0.1563) H88B(-0.2499) H88C(-
 0.2458) H90A(0.3267) H90B(0.4103) H90C(0.4133) H94A(0.6455) H94B(0.6894)
 H94C(0.5813) H96A(0.147) H96B(0.1185) H96C(0.1954) H10A(0.002) H10B(0.0602)
 H10C(0.0405) H10D(0.2822) H10E(0.3693) H10F(0.2713) H10G(0.7986) H10H(0.8034)
 H10I(0.7081) H10J(0.2221) H10K(0.2952) H10L(0.2149) H11D(0.5888) H11E(0.5598)
 H11F(0.4816) H11G(0.2373) H11H(0.2604) H11I(0.3417) H11A(0.1737) H11B(0.1602)
 H11C(0.2372) H12J(0.1445) H12K(0.131) H12L(0.1208) H12M(0.2502) H12N(0.1905)
 H12O(0.2912) H12A(-0.0116) H12B(0.0369) H12C(0.0896) H12D(0.1087) H12E(0.0618)
 H12F(0.0205) H13A(-0.0391) H13B(-0.0893) H13C(-0.0332) H13G(0.694)
 H13H(0.7367) H13I(0.7373) H13J(0.6297) H13K(0.7233) H13L(0.659) H13D(0.0778)
 H13E(0.0092) H13F(0.1184) H13M(0.3634) H13N(0.4331) H13O(0.4503) H14A(0.1016)
 H14B(0.0238) H14C(-0.0044) H14D(0.2697) H14E(0.3661) H14F(0.2753) H14J(0.611)
 H14K(0.5994) H14L(0.6287) H14G(0.1052) H14H(-0.0056) H14I(0.0437) H15A(-
 0.3256) H15B(-0.3613) H15C(-0.2875)
 Fixed Y: H17A(0.1268) H17B(0.0758) H17C(0.0676) H1A(0.4302) H1B(0.4476)
 H1C(0.3628) H4A(0.1736) H4B(0.1232) H4C(0.2126) H6A(0.2944) H6B(0.2426)
 H6C(0.2053) H7A(0.4395) H7B(0.4379) H7C(0.3914) H12G(0.0344) H12H(-0.0094)
 H12I(0.0738) H17D(0.425) H17E(0.5104) H17F(0.4792) H24A(0.2095) H24B(0.1201)
 H24C(0.1603) H28A(0.0881) H28B(0.11) H28C(0.1675) H29A(0.3211) H29B(0.3988)
 H29C(0.3913) H31A(0.255) H31B(0.3084) H31C(0.3108) H34A(0.4971) H34B(0.5307)
 H34C(0.5171) H36A(0.2959) H36B(0.2778) H36C(0.2905) H41A(0.1139) H41B(0.0317)
 H41C(0.1027) H45A(0.0368) H45B(0.055) H45C(0.1186) H48A(0.1386) H48B(0.1658)
 H48C(0.224) H54A(-0.0213) H54B(-0.1073) H54C(-0.0493) H56A(0.2563)
 H56B(0.1956) H56C(0.1929) H57A(0.3305) H57B(0.3574) H57C(0.2712) H60A(-0.0602)
 H60B(-0.0499) H60C(-0.0734) H63A(0.3924) H63B(0.3682) H63C(0.3059)
 H72A(0.1145) H72B(0.1688) H72C(0.2026) H74A(0.4114) H74B(0.4981) H74C(0.4352)
 H76A(0.2749) H76B(0.3226) H76C(0.2488) H78A(0.4528) H78B(0.4486) H78C(0.4827)
 H80A(0.373) H80B(0.4508) H80C(0.3782) H82A(0.2033) H82B(0.1829) H82C(0.2638)
 H84A(0.1602) H84B(0.1507) H84C(0.0885) H85A(0.5) H85B(0.5619) H85C(0.5125)
 H88A(0.1025) H88B(0.0533) H88C(0.1029) H90A(0.4067) H90B(0.4679) H90C(0.3836)
 H94A(0.0552) H94B(0.0612) H94C(0.036) H96A(-0.0802) H96B(-0.14) H96C(-0.0725)
 H10A(0.4643) H10B(0.515) H10C(0.4269) H10D(0.2926) H10E(0.2614) H10F(0.26)
 H10G(0.2292) H10H(0.3135) H10I(0.2614) H10J(0.5158) H10K(0.5535) H10L(0.4928)
 H11D(0.0428) H11E(-0.0288) H11F(0.0194) H11G(0.082) H11H(0.0673) H11I(0.0961)
 H11A(0.142) H11B(0.0856) H11C(0.0734) H12J(0.2417) H12K(0.1582) H12L(0.1726)
 H12M(0.271) H12N(0.2135) H12O(0.2477) H12A(0.1374) H12B(0.1665) H12C(0.1809)
 H12D(0.3207) H12E(0.3133) H12F(0.3656) H13A(0.3527) H13B(0.3752) H13C(0.4384)
 H13G(0.0984) H13H(0.1631) H13I(0.1763) H13J(0.3606) H13K(0.413) H13L(0.3854)
 H13D(0.4854) H13E(0.4354) H13F(0.4264) H13M(0.3897) H13N(0.4639) H13O(0.3958)
 H14A(-0.0323) H14B(-0.0994) H14C(-0.015) H14D(0.124) H14E(0.1164) H14F(0.0651)
 H14J(0.3876) H14K(0.4568) H14L(0.3792) H14G(0.29) H14H(0.2886) H14I(0.258)
 H15A(0.3335) H15B(0.4154) H15C(0.3882)
 Fixed Z: H17A(0.03) H17B(0.0375) H17C(0.0792) H1A(0.7816) H1B(0.7961)
 H1C(0.7804) H4A(0.8256) H4B(0.7516) H4C(0.7612) H6A(0.9854) H6B(1.0347)
 H6C(0.9619) H7A(0.2746) H7B(0.2205) H7C(0.2002) H12G(0.2394) H12H(0.2039)
 H12I(0.1933) H17D(0.3589) H17E(0.3965) H17F(0.3308) H24A(0.6959) H24B(0.6814)
 H24C(0.7154) H28A(0.1797) H28B(0.1351) H28C(0.2008) H29A(0.3355) H29B(0.3119)
 H29C(0.3602) H31A(0.6422) H31B(0.603) H31C(0.6028) H34A(0.9621) H34B(0.9152)
 H34C(0.8924) H36A(0.5242) H36B(0.597) H36C(0.5482) H41A(0.2342) H41B(0.247)
 H41C(0.3068) H45A(0.6391) H45B(0.5696) H45C(0.6362) H48A(-0.0291) H48B(-
 0.0354) H48C(-0.0005) H54A(0.7966) H54B(0.7793) H54C(0.7356) H56A(0.1031)
 H56B(0.0745) H56C(0.1447) H57A(0.4682) H57B(0.4139) H57C(0.4206) H60A(0.6206)
 H60B(0.5553) H60C(0.6178) H63A(0.7824) H63B(0.7167) H63C(0.7475) H72A(0.7424)
 H72B(0.7816) H72C(0.7433) H74A(0.9174) H74B(0.9198) H74C(0.8668) H76A(0.164)
 H76B(0.1899) H76C(0.2187) H78A(0.6543) H78B(0.6444) H78C(0.7166) H80A(0.0066)
 H80B(0.0445) H80C(0.026) H82A(0.4526) H82B(0.4877) H82C(0.4686) H84A(0.5576)
 H84B(0.6069) H84C(0.5408) H85A(0.7704) H85B(0.8238) H85C(0.7625) H88A(0.819)
 H88B(0.7849) H88C(0.8588) H90A(0.5079) H90B(0.5071) H90C(0.4682) H94A(0.0985)
 H94B(0.0305) H94C(0.0278) H96A(0.7569) H96B(0.8015) H96C(0.8324) H10A(0.8358)
 H10B(0.9011) H10C(0.8973) H10D(0.852) H10E(0.8896) H10F(0.919) H10G(0.2983)
 H10H(0.2857) H10I(0.2662) H10J(0.3928) H10K(0.4561) H10L(0.4645) H11D(0.3813)
 H11E(0.3227) H11F(0.3549) H11G(0.3139) H11H(0.3888) H11I(0.3499) H11A(0.6315)
 H11B(0.5604) H11C(0.6186) H12J(0.4049) H12K(0.4187) H12L(0.3431) H12M(0.1327)
 H12N(0.0722) H12O(0.0624) H12A(0.926) H12B(1.0013) H12C(0.9389) H12D(0.9778)
 H12E(1.0444) H12F(0.9954) H13A(0.6727) H13B(0.6063) H13C(0.664) H13G(0.5)
 H13H(0.5617) H13I(0.4861) H13J(0.3355) H13K(0.3633) H13L(0.4149) H13D(0.5924)
 H13E(0.532) H13F(0.5367) H13M(0.1489) H13N(0.167) H13O(0.2053) H14A(0.9312)
 H14B(0.9009) H14C(0.9167) H14D(0.9183) H14E(0.8871) H14F(0.8503) H14J(0.1728)
 H14K(0.1351) H14L(0.0955) H14G(0.5398) H14H(0.5283) H14I(0.5908) H15A(0.8907)
 H15B(0.9079) H15C(0.9604)
;
_shelx_res_checksum              30354
_olex2_date_sample_data_collection 2015-12-04
_olex2_submission_special_instructions 'No special instructions were received'