Square-Planar Alkylidyne-Osmium and Five-Coordinate Alkylidene-Osmium Complexes: Controlling the Transformation from Hydride-Alkylidyne to Alkylidene.
Buil, María L; Cardo, Juan J. F.; Esteruelas, Miguel A.; Oñate, Enrique; Journal of the American Chemical Society 138 (2016) 9720–9728; doi:10.1021/jacs.6b05825

data_4125160
_publ_section_title
;
 Square-Planar Alkylidyne-Osmium and Five-Coordinate Alkylidene-Osmium
 Complexes: Controlling the Transformation from Hydride-Alkylidyne to
 Alkylidene.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9720
_journal_page_last               9728
_journal_paper_doi               10.1021/jacs.6b05825
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '2(C43 H62 Cl N2 Os P), C5H12'
_chemical_formula_sum            'C45.5 H68 Cl N2 Os P'
_chemical_formula_weight         899.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.642(3)
_cell_length_b                   24.642(3)
_cell_length_c                   16.016(2)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     9725(2)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            103123
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.47
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    2.739
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.697
_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            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.033
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         12728
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+38.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                7669
_reflns_number_total             12728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b05825_si_003.cif
_cod_data_source_block           enriquen112d
_cod_depositor_comments
'Adding full bibliography for 4125159--4125160.cif.'
_cod_original_sg_symbol_H-M      P42/n
_cod_original_formula_sum        'C45.50 H68 Cl N2 Os P'
_cod_database_code               4125160