Amide-Directed Formation of Five-Coordinate Osmium Alkylidenes from Alkynes.
Casanova, Noelia; Esteruelas, Miguel A.; Gulías, Moisés; Larramona, Carmen; Mascareñas, José L; Oñate, Enrique; Organometallics 35 (2016) 91–99; doi:10.1021/acs.organomet.5b00777

data_4086364
_publ_section_title
;
 Amide-Directed Formation of Five-Coordinate Osmium Alkylidenes from
 Alkynes.
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              91
_journal_page_last               99
_journal_paper_doi               10.1021/acs.organomet.5b00777
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C29 H55 Cl2 N O Os P2, 2(CH2 Cl2)'
_chemical_formula_sum            'C31 H59 Cl6 N O Os P2'
_chemical_formula_weight         926.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.651(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.774(4)
_cell_length_b                   13.012(3)
_cell_length_c                   20.173(5)
_cell_measurement_reflns_used    5922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2.4
_cell_volume                     3987.0(17)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36954
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    3.705
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 7.56a (2008).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                7741
_reflns_number_total             10352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00777_si_001.cif
_cod_data_source_block           7-enriquen132
_cod_depositor_comments
;Adding full bibliography for 4086362--4086365.cif.

 Adding full bibliography for 4086362--4086365.cif.
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4086364