Multiple C−H Bond Activation of Phenyl-Substituted Pyrimidines and Triazines Promoted by an Osmium Polyhydride: Formation of Osmapolycycles with Three, Five, and Eight Fused Rings
Esteruelas, Miguel A.; Fernández, Israel; Herrera, Antonio; Martín-Ortiz, Mamen; Martínez-Álvarez, Roberto; Oliván, Montserrat; Oñate, Enrique; Sierra, Miguel A.; Valencia, Marta; Organometallics 29 (2010) 976–; doi:10.1021/om901030q

data_4067608
_publ_section_title
;
 Multiple C&#x2212;H Bond Activation of Phenyl-Substituted Pyrimidines and
 Triazines Promoted by an Osmium Polyhydride: Formation of Osmapolycycles
 with Three, Five, and Eight Fused Rings
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              976
_journal_paper_doi               10.1021/om901030q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C60 H105 N3 Os2 P4, C4 H10 O'
_chemical_formula_sum            'C64 H115 N3 O Os2 P4'
_chemical_formula_weight         1446.87
_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
_cell_angle_alpha                108.752(2)
_cell_angle_beta                 97.1420(10)
_cell_angle_gamma                92.741(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6776(2)
_cell_length_b                   15.1579(4)
_cell_length_c                   21.7645(3)
_cell_measurement_reflns_used    23413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6805
_cell_measurement_theta_min      2.8790
_cell_volume                     3295.24(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details
;
  1 omega    0.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177   45.0000   90.0000    0.0000    0.0000 51

  2 omega    0.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -77.0000   30.0000    0.0000    0.0000 55

  3 omega  -51.00    1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000  150.0000    0.0000    0.0000 52

  4 omega  -11.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   77.0000  300.0000    0.0000    0.0000 55

  5 omega   -3.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865  -45.0000  330.0000    0.0000    0.0000 52

  6 omega  -11.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865   77.0000  150.0000    0.0000    0.0000 55

  7 omega   20.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865    0.0000   90.0000    0.0000    0.0000 77

  8 omega  -96.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -21.1177    0.0000    0.0000    0.0000    0.0000 150

  9 omega  -53.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865    0.0000    0.0000    0.0000    0.0000 150

 10 omega  -53.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865    0.0000  240.0000    0.0000    0.0000 150

 11 omega  -53.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865    0.0000  180.0000    0.0000    0.0000 150

 12 omega  -53.00  -16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       21.5865    0.0000   60.0000    0.0000    0.0000 37

;
_diffrn_measurement_device_type
;
Oxford Diffraction Excalibur (TM) single-crystal X-ray diffractometer
with Sapphire CCD detector
;
_diffrn_measurement_method
;
Rotation method data acquisition using \w and \q
;
_diffrn_orient_matrix_UB_11      -0.0206157076
_diffrn_orient_matrix_UB_12      0.0427584405
_diffrn_orient_matrix_UB_13      -0.0024567776
_diffrn_orient_matrix_UB_21      -0.0519704726
_diffrn_orient_matrix_UB_22      -0.0050460147
_diffrn_orient_matrix_UB_23      0.0163867832
_diffrn_orient_matrix_UB_31      0.0374377853
_diffrn_orient_matrix_UB_32      0.0247760324
_diffrn_orient_matrix_UB_33      0.0306291831
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62671
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    3.990
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         14417
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                9735
_reflns_number_total             14417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901030q_si_002.cif
_cod_data_source_block           est1
_cod_database_code               4067608