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_1551049
_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 N O13 Si3'
_chemical_formula_sum            'C36 H81 Mo N O13 Si3'
_chemical_formula_weight         916.22
_chemical_name_systematic        '[Mo(NO)(TBOS)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             2017-09-19
_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                 90.002(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.0970(3)
_cell_length_b                   46.8142(14)
_cell_length_c                   23.0986(5)
_cell_measurement_reflns_used    15165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4240
_cell_measurement_theta_min      2.8626
_cell_volume                     15243.7(6)
_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  -95.00   -2.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827  -57.0000    0.0000 124

  2 omega  -25.00   20.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827  -99.0000  -60.0000 60

  3 omega  -48.00   45.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827   57.0000  150.0000 124

  4 omega  -20.50   20.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827  -99.0000  150.0000 54

  5 omega   -2.00   94.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -       25.0515   38.0000  -60.0000 128

  6 omega -104.00  -74.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827 -179.0000  120.0000 40

  7 omega  -56.00   49.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.5827   38.0000    0.0000 140
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0088734000
_diffrn_orient_matrix_UB_12      -0.0148345000
_diffrn_orient_matrix_UB_13      0.0030178000
_diffrn_orient_matrix_UB_21      -0.0476465000
_diffrn_orient_matrix_UB_22      -0.0029823000
_diffrn_orient_matrix_UB_23      -0.0077988000
_diffrn_orient_matrix_UB_31      0.0134613000
_diffrn_orient_matrix_UB_32      -0.0007424000
_diffrn_orient_matrix_UB_33      -0.0295637000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            117825
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.868
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.987
_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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       plate
_exptl_crystal_F_000             5904
_exptl_crystal_preparation       'reaction of Mo(silox)3 with N2O'
_exptl_crystal_recrystallization_method
'crystallized through slow evaporation of a pentane solution at - 40 degrees Celsius'
_exptl_crystal_size_max          0.6924
_exptl_crystal_size_mid          0.3017
_exptl_crystal_size_min          0.0517
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1572
_refine_ls_number_reflns         26891
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0109P)^2^+55.7612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19929
_reflns_number_total             26891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           mp-n2o
_cod_database_code               1551049
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Mo1 Si3 O12 C40 H40 N2'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9968(2)
 0.0032(2)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C41, C44B, C43A, C44A, C42B, C42A, C43B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C44B)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C42B)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C43B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(1)
 Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C43A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(1)
6.a Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C98(H98A,H98B,H98C), C64(H64A,H64B,H64C), C106(H10D,H10E,
 H10F), C86(H86A,H86B,H86C), C75(H75A,H75B,H75C), C62(H62A,H62B,H62C), C79(H79A,
 H79B,H79C), C100(H10G,H10H,H10I), C71(H71A,H71B,H71C), C26(H26A,H26B,H26C),
 C88(H88A,H88B,H88C), C108(H10J,H10K,H10L), C3(H3A,H3B,H3C), C16(H16A,H16B,
 H16C), C87(H87A,H87B,H87C), C46(H46A,H46B,H46C), C63(H63A,H63B,H63C), C48(H48A,
 H48B,H48C), C102(H10M,H10N,H10O), C8(H8A,H8B,H8C), C55(H55A,H55B,H55C),
 C99(H99A,H99B,H99C), C104(H10P,H10Q,H10R), C12(H12A,H12B,H12C), C2(H2A,H2B,
 H2C), C28(H28A,H28B,H28C), C68(H68A,H68B,H68C), C15(H15A,H15B,H15C), C30(H30A,
 H30B,H30C), C23(H23A,H23B,H23C), C84(H84A,H84B,H84C), C103(H10S,H10T,H10U),
 C47(H47A,H47B,H47C), C80(H80A,H80B,H80C), C67(H67A,H67B,H67C), C70(H70A,H70B,
 H70C), C74(H74A,H74B,H74C), C107(H10V,H10W,H10X), C83(H83A,H83B,H83C),
 C58(H58A,H58B,H58C), C90(H90A,H90B,H90C), C94(H94A,H94B,H94C), C18(H18A,H18B,
 H18C), C56(H56A,H56B,H56C), C92(H92A,H92B,H92C), C31(H31A,H31B,H31C), C82(H82A,
 H82B,H82C), C34(H34A,H34B,H34C), C72(H72A,H72B,H72C), C11(H11A,H11B,H11C),
 C32(H32A,H32B,H32C), C14(H14A,H14B,H14C), C66(H66A,H66B,H66C), C76(H76A,H76B,
 H76C), C36(H36A,H36B,H36C), C19(H19A,H19B,H19C), C91(H91A,H91B,H91C), C10(H10A,
 H10B,H10C), C54(H54A,H54B,H54C), C24(H24A,H24B,H24C), C4(H4A,H4B,H4C),
 C59(H59A,H59B,H59C), C6(H6A,H6B,H6C), C38(H38A,H38B,H38C), C78(H78A,H78B,H78C),
  C52(H52A,H52B,H52C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C95(H95A,H95B,
 H95C), C35(H35A,H35B,H35C), C50(H50A,H50B,H50C), C7(H7A,H7B,H7C), C40(H40A,
 H40B,H40C), C60(H60A,H60B,H60C), C96(H96A,H96B,H96C), C51(H51A,H51B,H51C),
 C44B(H44A,H44B,H44C), C39(H39A,H39B,H39C), C42B(H42A,H42B,H42C), C42A(H42D,
 H42E,H42F), C44A(H44D,H44E,H44F), C43B(H43A,H43B,H43C), C43A(H43D,H43E,H43F)
;
_olex2_date_sample_data_collection 2016-02-15
_olex2_exptl_crystal_mounting_method 'mounted in paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'