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_1551046
_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 H87 Mo O12 Si3'
_chemical_formula_sum            'C40 H87 Mo O12 Si3'
_chemical_formula_weight         940.30
_chemical_name_systematic        '[Mo(C4H6)(OSi(OtBu)3)3]'
_chemical_properties_physical    Air-sensitive,Heat-sensitive,Oxygen-sensitive
_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                 108.995(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5671(15)
_cell_length_b                   21.407(2)
_cell_length_c                   19.204(2)
_cell_measurement_reflns_used    4764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.21
_cell_volume                     5273.7(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.091
_diffrn_reflns_theta_max         25.091
_diffrn_reflns_theta_min         1.471
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0737 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.8215.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_preparation       'reaction of Mo[OSi(OtBu)3]3 with 2-butyne'
_exptl_crystal_recrystallization_method
'slow evaporation of a pentane solution'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0641P)^2^+3.7293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6803
_reflns_number_total             9365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           mo
_cod_original_cell_volume        5273.8(10)
_cod_database_code               1551046
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C),
 C15(H15A,H15B,H15C), C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C28(H28A,H28B,
 H28C), C11(H11A,H11B,H11C), C37(H37A,H37B,H37C), C14(H14A,H14B,H14C), C8(H8A,
 H8B,H8C), C6(H6A,H6B,H6C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C31(H31A,
 H31B,H31C), C3(H3A,H3B,H3C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C),
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C18(H18A,H18B,
 H18C), C36(H36A,H36B,H36C), C26(H26A,H26B,H26C), C20(H20A,H20B,H20C), C24(H24A,
 H24B,H24C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'