Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with Different Ring Size†,1
Lindner, Ekkehard; Krebs, Ilmari; Fawzi, Riad; Steimann, Manfred; Speiser, Bernd; Organometallics 18 (1999) 480–; doi:10.1021/om980713e

data_4077737
_publ_section_title
;
 Synthesis, Structure, and Electrochemistry of Osmametallocenophanes with
 Different Ring Size&#x2020;,1
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              480
_journal_paper_doi               10.1021/om980713e
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C26 H32 O4 Os Ru'
_chemical_formula_weight         699.79
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.901(3)
_cell_length_b                   49.915(11)
_cell_length_c                   9.112(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      15
_cell_volume                     2543.1(16)
_computing_cell_refinement       '&#x00B4;Xscans V2.20&#x00B4;'
_computing_data_collection       '&#x00B4;Xscans V2.20&#x00B4;'
_computing_data_reduction        '&#x00B4;Xscans V2.20&#x00B4;'
_computing_molecular_graphics    '&#x00B4;XP &#x00B4;'
_computing_publication_material  '&#x00B4;XCIF &#x00B4;'
_computing_structure_refinement  'SHELXTL-5.03 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXTL-5.03 (Sheldrick, 1995)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       '&#x00B4;Siemens P4&#x00B4;'
_diffrn_measurement_method       '&#x00B4;Omega Scan&#x00B4;'
_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  0.1344
_diffrn_reflns_av_sigmaI/netI    0.1369
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9064
_diffrn_reflns_theta_max         44.11
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.613
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            cube
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.422
_refine_diff_density_min         -2.840
_refine_diff_density_rms         0.340
_refine_ls_extinction_coef       0.0006(4)
_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_all   2.231
_refine_ls_goodness_of_fit_obs   2.088
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.450
_refine_ls_restrained_S_obs      2.088
_refine_ls_R_factor_all          0.1660
_refine_ls_R_factor_obs          0.0904
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc 
 [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+135.1239*P+(0.0493P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_wR_factor_all         0.2935
_refine_ls_wR_factor_obs         0.2061
_reflns_number_observed          3015
_reflns_number_total             4467
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980713e.cif
_cod_data_source_block           krebs_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Psi-Scan' changed to
'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2543.1(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077737