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_1551051
_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         'C40 H89 Mo O12 Si3'
_chemical_formula_sum            'C40 H89 Mo O12 Si3'
_chemical_formula_weight         942.32
_chemical_name_systematic        '[Mo(C4H8)(OSi(OtBu)3)3]'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 150.1(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.388(19)
_cell_length_b                   22.712(6)
_cell_length_c                   26.40(3)
_cell_measurement_reflns_used    884
_cell_measurement_temperature    104(4)
_cell_measurement_theta_max      30.5419
_cell_measurement_theta_min      2.9280
_cell_volume                     5496(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      104(4)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.9757
_diffrn_measured_fraction_theta_max 0.9461
_diffrn_measurement_details
;
  1 omega  -98.00  -47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904 -179.0000  150.0000 51

  2 omega  -25.00  -14.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   30.0000 11
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0496676000
_diffrn_orient_matrix_UB_12      0.0108605000
_diffrn_orient_matrix_UB_13      0.0116672000
_diffrn_orient_matrix_UB_21      -0.0258011000
_diffrn_orient_matrix_UB_22      0.0290828000
_diffrn_orient_matrix_UB_23      -0.0112639000
_diffrn_orient_matrix_UB_31      0.0531498000
_diffrn_orient_matrix_UB_32      0.0038705000
_diffrn_orient_matrix_UB_33      0.0512967000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.1371
_diffrn_reflns_Laue_measured_fraction_full 0.9757
_diffrn_reflns_Laue_measured_fraction_max 0.9461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6209
_diffrn_reflns_point_group_measured_fraction_full 0.9757
_diffrn_reflns_point_group_measured_fraction_max 0.9461
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91241
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         5377
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0908
_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^)+(0.0540P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3475
_reflns_number_total             5377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           vmmosilox
_cod_original_cell_volume        5496(25)
_cod_database_code               1551051
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'Mo1 Si3 O12 C36 H81'
_reflns_odcompleteness_completeness 44.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O7B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) = Uanis(C37B) = Uanis(C40B) = Uanis(C39B) = Uanis(C38B)
Uanis(C37) = Uanis(C40) = Uanis(C38) = Uanis(C39) = Uanis(O7B)
Uanis(O7B) = Uanis(Si2)
3. Others
 Sof(C37B)=Sof(C40B)=Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C38B)=Sof(H38D)=
 Sof(H38E)=Sof(H38F)=Sof(C39B)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(O8)=1-FVAR(1)
 Sof(O7B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C40)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C37)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C31(H31A,H31B,H31C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C6(H6A,
 H6B,H6C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C16(H16A,
 H16B,H16C), C24(H24A,H24B,H24C), C34(H34A,H34B,H34C), C15(H15A,H15B,H15C),
 C26(H26A,H26B,H26C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C19(H19A,H19B,H19C),
  C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C), C22(H22A,H22B,
 H22C), C40B(H40A,H40B,H40C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C3(H3A,
 H3B,H3C), C4(H4A,H4B,H4C), C38B(H38D,H38E,H38F), C39B(H39A,H39B,H39C),
 C39(H39D,H39E,H39F), C40(H40D,H40E,H40F)
;
_olex2_date_sample_data_collection 2015-10-29
_olex2_submission_special_instructions 'No special instructions were received'