A Mo(VI) Alkylidyne Complex with Polyhedral Oligomeric Silsesquioxane Ligands: Homogeneous Analogue of a Silica-Supported Alkyne Metathesis Catalyst
Hyeon Mo Cho; Haim Weissman; Scott R. Wilson; Jeffrey S. Moore; Journal of the American Chemical Society 128 (2006) 14742–14743; doi:10.1021/ja065101x

data_4111094
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 A Mo(VI) Alkylidyne Complex with Polyhedral Oligomeric Silsesquioxane
 Ligands: Homogeneous Analogue of a Silica-Supported Alkyne Metathesis
 Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14742
_journal_page_last               14743
_journal_paper_doi               10.1021/ja065101x
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C97 H168 Mo N2 O26 Si16'
_chemical_formula_sum            'C97 H168 Mo N2 O26 Si16'
_chemical_formula_weight         2323.71
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2006-06-21   text and data added, hmc 
;
_cell_angle_alpha                79.785(2)
_cell_angle_beta                 82.574(2)
_cell_angle_gamma                82.006(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1440(6)
_cell_length_b                   14.0403(8)
_cell_length_c                   20.9983(12)
_cell_measurement_reflns_used    5194
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      17.82
_cell_measurement_theta_min      2.26
_cell_volume                     3183.5(3)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga63isax
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41795
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1238
_exptl_crystal_id                ga63isax
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.4 mm cryo-loop (Hampton Research) with the (6 3 2) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.682
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         6661
_refine_ls_number_restraints     1652
_refine_ls_restrained_S_all      1.769
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.1241
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3446
_refine_ls_wR_factor_ref         0.3908
_reflns_number_gt                3311
_reflns_number_total             6661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065101xsi20060725_042431.cif
_cod_data_source_block           ga63isax
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4111094