Dihydride versus Elongated Dihydrogen in [H2Os(κ2-O2CCH3)L(PiPr3)2]+Complexes: Influence of the L Ligand
Esteruelas, Miguel A.; García-Yebra, Cristina; Oliván, Montserrat; Oñate, Enrique; Tajada, María A.; Organometallics 21 (2002) 1311–; doi:10.1021/om010891z

data_4076663
_publ_section_title
;
 Dihydride versus Elongated Dihydrogen in
 [H2Os(\k2-O2CCH3)L(PiPr3)2]+Complexes:&#x00A0; Influence of the L Ligand
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1311
_journal_paper_doi               10.1021/om010891z
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C23 H56 B F4 O5 Os P3'
_chemical_formula_weight         782.60
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.541(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3503(13)
_cell_length_b                   21.666(3)
_cell_length_c                   13.7786(16)
_cell_measurement_reflns_used    4037
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     3307.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_type            'Bruker SMART APEX'
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type
;
'three-circle diffractometer with CCD area detector'
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30560
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.052
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7959
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.275
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                4786
_reflns_number_total             7959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010891z.cif
_cod_data_source_block           mae35as
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076663