Reactions of Osmium Hydrido Alkenylcarbyne with Allenoates: Insertion and [3 + 2] Annulation
Zhou, Xiaoxi; He, Xiehua; Lin, Jianfeng; Zhuo, Qingde; Chen, Zhixin; Zhang, Hong; Wang, Jianbo; Xia, Haiping; Organometallics 34 (2015) 1742–; doi:10.1021/acs.organomet.5b00242

data_4087539
_publ_section_title
;
 Reactions of Osmium Hydrido Alkenylcarbyne with Allenoates: Insertion and
 [3 + 2] Annulation
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1742
_journal_paper_doi               10.1021/acs.organomet.5b00242
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C75 H67 O4 Os P3, 3(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C78 H73 B2 Cl6 F8 O4 Os P3'
_chemical_formula_weight         1743.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                70.9680(10)
_cell_angle_beta                 88.3510(10)
_cell_angle_gamma                79.5320(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4738(4)
_cell_length_b                   16.1429(5)
_cell_length_c                   20.2952(7)
_cell_measurement_temperature    173
_cell_volume                     3797.0(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28619
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.906
_refine_diff_density_min         -5.521
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         13123
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1610P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2026
_refine_ls_wR_factor_ref         0.2984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8016
_reflns_number_total             13123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00242_si_003.cif
_cod_data_source_block           complex_3
_cod_database_code               4087539
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C10, C1, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C216) = Uanis(C211) = Uanis(C212) = Uanis(C213) = Uanis(C214) =
Uanis(C215)
4.a Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C14(H14a,H14b), C20(H20a,H20b), C3S(H3Sa,H3Sb), C2S(H2Sa,
 H2Sb), C1S(H1Sa,H1Sb)
4.b Me refined with riding coordinates:
 C21(H21a,H21b,H21c), C15(H15a,H15b,H15c)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C332(H332), C124(H124), C12(H12), C322(H322), C212(H212),
 C216(H216), C126(H126), C132(H132), C10(H10), C113(H113), C114(H114),
 C122(H122), C326(H326), C125(H125), C226(H226), C5(H5), C135(H135), C224(H224),
  C234(H234), C236(H236), C336(H336), C136(H136), C116(H116), C3(H3),
 C316(H316), C9(H9), C112(H112), C6(H6), C222(H222), C324(H324), C215(H215),
 C314(H314), C115(H115), C134(H134), C335(H335), C325(H325), C333(H333),
 C312(H312), C213(H213), C223(H223), C323(H323), C232(H232), C214(H214),
 C315(H315), C133(H133), C225(H225), C8(H8), C235(H235), C233(H233), C7(H7),
 C313(H313), C334(H334), C123(H123)
;
_olex2_submission_special_instructions 'No special instructions were received'