Orientational isomerism in bridging 2-pyridyl complexes: orthometallation of (S )-nicotine and (R)-1-(4-pyridyl)ethanol in triosmium clusters
Deeming, Antony J.; Stchedroff, Marc J.; Whittaker, Caroline; Arce, Alejandro J.; De Sanctis, Ysaura; Steed, Jonathan W.; Journal of the Chemical Society, Dalton Transactions  (1999) 3289–; doi:10.1039/a902061f

data_7027388
_publ_section_title
;
 Orientational isomerism in bridging 2-pyridyl complexes: orthometallation
 of (S&#x200A;)-nicotine and (R)-1-(4-pyridyl)ethanol in triosmium
 clusters
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3289
_journal_paper_doi               10.1039/a902061f
_journal_year                    1999
_chemical_formula_sum            'C19 H9 N O11 Os3'
_chemical_formula_weight         997.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 93.680(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9372(11)
_cell_length_b                   11.7406(8)
_cell_length_c                   9.1656(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2355.8(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Xseed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '2o phi prames + omega to complete'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14598
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    16.199
_exptl_absorpt_correction_T_max  0.4432
_exptl_absorpt_correction_T_min  0.1400
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.731
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.250
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(19)
_refine_ls_extinction_coef       0.00037(6)
_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   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5017
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+48.9326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                4856
_reflns_number_total             5017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            902061Fsup1.cif
_cod_data_source_block           os3mepy
_cod_original_cell_volume        2355.8(8)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7027388