POP-Pincer Osmium-Polyhydrides: Head-to-Head (Z)-Dimerization of Terminal Alkynes
Joaquín Alós; Tamara Bolaño; Miguel A. Esteruelas; Montserrat Oliván; Enrique Oñate; Marta Valencia; Inorganic Chemistry 52 (2013) 6199–6213; doi:10.1021/ic400730a

data_4334976
_publ_contact_author
;
  Dr. Enrique O\~nate 
  Departamento de Qu\'imica Inorg\'anica - ISQCH
  Facultad de Ciencias
  Universidad de Zaragoza - CSIC
  50009 Zaragoza, Spain
;
_publ_contact_author_email       enriqueo@unizar.es
_publ_section_title
;
 POP-Pincer Osmium-Polyhydrides: Head-to-Head (Z)-Dimerization of Terminal
 Alkynes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6199
_journal_page_last               6213
_journal_paper_doi               10.1021/ic400730a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C31 H51 Cl2 O2.5 Os P2 S'
_chemical_formula_weight         818.82
_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                 94.263(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.775(2)
_cell_length_b                   13.0623(18)
_cell_length_c                   27.771(4)
_cell_measurement_reflns_used    5442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6791.8(15)
_computing_cell_refinement       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_reduction
;
  SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS
;
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker SMART 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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            42941
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.603
_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. 6.1 (2000).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       needle
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     738
_refine_ls_number_reflns         15626
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                10404
_reflns_number_total             15626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400730a_si_002_2.cif
_cod_data_source_block           montse5as
_cod_original_cell_volume        6792.1(15)
_cod_original_formula_sum        'C31 H51 Cl2 O2.50 Os P2 S'
_cod_database_code               4334976