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_4334977
_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            'C27 H43 Cl O Os P2'
_chemical_formula_weight         671.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.788(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.13(2)
_cell_length_b                   12.148(7)
_cell_length_c                   14.516(8)
_cell_measurement_reflns_used    9418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     5752(6)
_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 0.996
_diffrn_measured_fraction_theta_max 0.934
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34295
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.702
_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            colorless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       prism
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.347
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+5.9972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                5879
_reflns_number_total             6929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400730a_si_002_3.cif
_cod_data_source_block           montse6as
_cod_database_code               4334977