Silica-supported isolated molybdenum di-oxo species: formation and activation with organosilicon agent for olefin metathesis.
Yamamoto, Keishi; Chan, Ka Wing; Mougel, Victor; Nagae, Haruki; Tsurugi, Hayato; Safonova, Olga V.; Mashima, Kazushi; Copéret, Christophe; Chemical communications (Cambridge, England) 54 (2018) 3989–3992; doi:10.1039/c8cc01876f

data_7121440
_publ_section_title
;
 Silica-supported isolated molybdenum di-oxo species: formation and
 activation with organosilicon agent for olefin metathesis.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3989
_journal_page_last               3992
_journal_paper_doi               10.1039/c8cc01876f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 H54 Mo O10 Si2'
_chemical_formula_sum            'C24 H54 Mo O10 Si2'
_chemical_formula_weight         654.79
_chemical_name_systematic        Mo(silox)2O2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.232(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.151(5)
_cell_length_b                   27.037(8)
_cell_length_c                   16.893(5)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.24
_cell_volume                     7006(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0993
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36518
_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         1.327
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1498 before and 0.0626 after correction.
The Ratio of minimum to maximum transmission is 0.7063.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       needle
_exptl_crystal_F_000             2784
_exptl_crystal_preparation       'reaction of Mo(silox)3 with O2'
_exptl_crystal_recrystallization_method
'slow evaporation of a pentane solution at -40 degrees celsius'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0432P)^2^+5.7438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7302
_reflns_number_total             12370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01876f3.cif
_cod_data_source_block           mo
_cod_depositor_comments          'Adding full bibliography for 7121440.cif.'
_cod_original_cell_volume        7006(3)
_cod_database_code               7121440
_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:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C46(H46A,H46B,H46C), C8(H8A,H8B,
 H8C), C24(H24A,H24B,H24C), C7(H7A,H7B,H7C), C47(H47A,H47B,H47C), C19(H19A,H19B,
 H19C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C12(H12A,H12B,
 H12C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C35(H35A,H35B,H35C), C22(H22A,
 H22B,H22C), C20(H20A,H20B,H20C), C43(H43A,H43B,H43C), C32(H32A,H32B,H32C),
 C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C16(H16A,H16B,H16C), C14(H14A,H14B,
 H14C), C26(H26A,H26B,H26C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C34(H34A,
 H34B,H34C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C2(H2A,
 H2B,H2C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C30(H30A,H30B,H30C),
 C40(H40A,H40B,H40C), C39(H39A,H39B,H39C)
;
_olex2_exptl_crystal_mounting_method 'mounted in paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'