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_1551047
_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         'C72 H162 Mo2 N2 O24 Si6'
_chemical_formula_sum            'C72 H162 Mo2 N2 O24 Si6'
_chemical_formula_weight         1800.45
_chemical_name_systematic        (\m-N2)[Mo(TBOS)3]2
_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                 98.374(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3543(9)
_cell_length_b                   22.6953(16)
_cell_length_c                   30.713(2)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.30
_cell_volume                     9898.9(11)
_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      103.6
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            133726
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.113
_diffrn_reflns_theta_min         2.240
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.7384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0888 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.8566.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             3872
_exptl_crystal_preparation       'reaction with N2'
_exptl_crystal_recrystallization_method
'slow evaporation of a pentane solution at -40 degrees celsius'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00057(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         19472
_refine_ls_number_restraints     1047
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0689P)^2^+27.6095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12461
_reflns_number_total             19472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01955c2.cif
_cod_data_source_block           mon2
_cod_database_code               1551047
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O23B)=Sof(O22A)=Sof(C61A)=Sof(C69B)=Sof(O24A)=Sof(C65B)=Sof(C64A)=
 Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=
 Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C68B)=Sof(H68A)=Sof(H68B)=
 Sof(H68C)=Sof(C67B)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C66B)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=Sof(C72B)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C70B)=
 Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C71B)=Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(1)
 Sof(O24B)=Sof(C65A)=Sof(O22B)=Sof(O0AA)=Sof(C61B)=Sof(C69A)=Sof(C63B)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C62B)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C64B)=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C67A)=Sof(H67A)=Sof(H67B)=
 Sof(H67C)=Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(C68A)=Sof(H68D)=
 Sof(H68E)=Sof(H68F)=Sof(C71A)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72A)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=FVAR(1)
4.a Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C54(H54A,H54B,H54C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C), C56(H56A,H56B,H56C), C27(H27A,
 H27B,H27C), C22(H22A,H22B,H22C), C58(H58A,H58B,H58C), C20(H20A,H20B,H20C),
 C38(H38A,H38B,H38C), C24(H24A,H24B,H24C), C40(H40A,H40B,H40C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C55(H55A,H55B,H55C), C48(H48A,H48B,H48C), C36(H36A,
 H36B,H36C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C39(H39A,H39B,H39C),
 C18(H18A,H18B,H18C), C34(H34A,H34B,H34C), C11(H11A,H11B,H11C), C42(H42A,H42B,
 H42C), C2(H2A,H2B,H2C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C),
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C19(H19A,H19B,H19C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C44(H44A,H44B,
 H44C), C4(H4A,H4B,H4C), C43(H43A,H43B,H43C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C64A(H64A,H64B,H64C), C63B(H63A,H63B,H63C), C62B(H62A,H62B,H62C),
 C63A(H63D,H63E,H63F), C62A(H62D,H62E,H62F), C64B(H64D,H64E,H64F), C68B(H68A,
 H68B,H68C), C67A(H67A,H67B,H67C), C67B(H67D,H67E,H67F), C66B(H66A,H66B,H66C),
 C66A(H66D,H66E,H66F), C68A(H68D,H68E,H68F), C72B(H72A,H72B,H72C), C71A(H71A,
 H71B,H71C), C70B(H70A,H70B,H70C), C72A(H72D,H72E,H72F), C71B(H71D,H71E,H71F),
 C70A(H70D,H70E,H70F)
;
_olex2_exptl_crystal_mounting_method 'mounted in oil'
_olex2_submission_special_instructions 'No special instructions were received'