Osmium−Alkenylcarbyne and −Alkenylcarbene Complexes with an Steroid Skeleton: Formation of a Testosterone Organometallic Derivative Containing the 7H-Amino Adenine Tautomer
Buil, María L.; Esteruelas, Miguel A.; Garcés, Karin; Oñate, Enrique; Organometallics 28 (2009) 5691–; doi:10.1021/om900647a

data_4070205
_publ_section_title
;
 Osmium&#x2212;Alkenylcarbyne and &#x2212;Alkenylcarbene Complexes with an
 Steroid Skeleton: Formation of a Testosterone Organometallic Derivative
 Containing the 7H-Amino Adenine Tautomer
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5691
_journal_paper_doi               10.1021/om900647a
_journal_volume                  28
_journal_year                    2009
_chemical_absolute_configuration rm
_chemical_formula_sum            'C48.45 H85.9 Cl1.9 F6 N5 O2 Os P3'
_chemical_formula_weight         1234.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.375(3)
_cell_angle_beta                 93.131(3)
_cell_angle_gamma                97.394(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3170(16)
_cell_length_b                   16.066(2)
_cell_length_c                   18.498(3)
_cell_measurement_reflns_used    4839
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     3129.4(8)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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      223(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.909
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.1269
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39237
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    2.213
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
XPREP, SHELXTL v. 6.1 (Bruker, 2000)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.880
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.110(11)
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1200
_refine_ls_number_reflns         28335
_refine_ls_number_restraints     936
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2313
_reflns_number_gt                18408
_reflns_number_total             28335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900647a_si_002.cif
_cod_data_source_block           mae413bs
_cod_original_cell_volume        3129.3(8)
_cod_original_formula_sum        'C48.45 H85.90 Cl1.90 F6 N5 O2 Os P3'
_cod_database_code               4070205