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_1551054
_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 Mo N O12 Si3'
_chemical_formula_sum            'C36 Mo N O12 Si3'
_chemical_formula_weight         818.58
_chemical_name_systematic        '[Mo(N)(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_primary     direct
_audit_creation_date             2016-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-03-01 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                81.009(5)
_cell_angle_beta                 85.125(4)
_cell_angle_gamma                89.850(4)
_cell_formula_units_Z            8
_cell_length_a                   13.8093(7)
_cell_length_b                   23.8436(13)
_cell_length_c                   31.3560(16)
_cell_measurement_reflns_used    4809
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      29.4652
_cell_measurement_theta_min      2.8205
_cell_volume                     10160.0(9)
_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
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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      103(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details
;
  1 omega  -24.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0055  -99.0000 -180.0000 46

  2 omega  -25.00   22.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0055  -99.0000    0.0000 47

  3 omega   34.00  100.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4742  179.0000 -150.0000 66

  4 omega   -2.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4742   49.0000  -23.0000 95

  5 omega  -19.00   89.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4742   19.0000  -90.0000 108

  6 omega  -51.00   49.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       21.4742  -38.0000 -120.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0060839000
_diffrn_orient_matrix_UB_12      0.0010601000
_diffrn_orient_matrix_UB_13      -0.0228034000
_diffrn_orient_matrix_UB_21      0.0469289000
_diffrn_orient_matrix_UB_22      0.0122131000
_diffrn_orient_matrix_UB_23      -0.0004534000
_diffrn_orient_matrix_UB_31      0.0204552000
_diffrn_orient_matrix_UB_32      -0.0275123000
_diffrn_orient_matrix_UB_33      0.0028616000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1662
_diffrn_reflns_av_unetI/netI     0.3709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            82779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.826
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.989
_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_density_diffrn    1.070
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.2953
_exptl_crystal_size_mid          0.1696
_exptl_crystal_size_min          0.1165
_refine_diff_density_max         2.239
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1910
_refine_ls_number_reflns         41254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.3459
_refine_ls_R_factor_gt           0.1506
_refine_ls_shift/su_max          0.484
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3570
_refine_ls_wR_factor_ref         0.4874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12156
_reflns_number_total             41254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           mp-mon2
_cod_database_code               1551054
_chemical_oxdiff_formula         'Mo1 Si3 O12 C50 H80 N2'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.931(2) 0.069(2)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-17
_olex2_submission_special_instructions 'No special instructions were received'