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_1551050
_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         'C38 H85 Mo O12 Si3'
_chemical_formula_sum            'C38 H85 Mo O12 Si3'
_chemical_formula_weight         914.26
_chemical_name_systematic        '[Mo(C2H4)(OSi(OtBu)3)3]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-18
_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                 90.757(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2016(4)
_cell_length_b                   22.5836(8)
_cell_length_c                   24.6875(8)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7751
_cell_measurement_theta_min      2.8500
_cell_volume                     5129.7(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -44.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8873   77.0000  150.0000 95

  2 omega  -25.00   21.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8873  -98.0000  -80.0000 46

  3 omega  -86.00    2.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8873  -38.0000 -150.0000 88

  4 omega  -84.00   10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8873  -77.0000   30.0000 94

  5 omega  -44.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8873   77.0000  -30.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.856
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   analytical
_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)
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)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_preparation       'Reaction of Mo[OSI(OtBu)3]3 with ethylene'
_exptl_crystal_recrystallization_method
'Slow evaporation of a pentane solution at -40 degrees'
_exptl_crystal_size_max          0.4964
_exptl_crystal_size_mid          0.3167
_exptl_crystal_size_min          0.2272
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         11305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0090P)^2^+16.6843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8094
_reflns_number_total             11305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           mp-moethylene
_cod_original_cell_volume        5129.8(3)
_cod_database_code               1551050
_shelx_shelxl_version_number     2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C33(H33A,
 H33B,H33C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C30(H30A,H30B,H30C),
 C25(H25A,H25B,H25C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C20(H20A,H20B,
 H20C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C),
 C38(H38A,H38B,H38C), C21(H21A,H21B,H21C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C),
  C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C)
;
_olex2_exptl_crystal_mounting_method 'Mounted in paratone'
_olex2_submission_special_instructions 'No special instructions were received'