Substitution Reactions of aμ3-η1:η2:η1-C60Triosmium Cluster Complex and Formation of a Novelμ3-η1:η1:η2-C60Bonding Mode
Song, Hyunjoon; Choi, Jae Ik; Lee, Kwangyeol; Choi, Moon-Gun; Park, Joon T.; Organometallics 21 (2002) 5221–; doi:10.1021/om0205703

data_4077086
_publ_section_title
;
 Substitution Reactions of a\m3-\h1:\h2:\h1-C60Triosmium Cluster Complex
 and Formation of a Novel\m3-\h1:\h1:\h2-C60Bonding Mode
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5221
_journal_paper_doi               10.1021/om0205703
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety
'Os3(CO)7(CNCH2Ph)2(mu3-CNCH2Ph)(mu3-eta1:eta2:eta1-C60).C6H4Cl2 (3.C6H4Cl2)'
_chemical_formula_sum            'C97 H25 Cl2 N3 O7 Os3'
_chemical_formula_weight         1985.70
_chemical_name_systematic
; 
 Os3(CO)7(CNCH2Ph)2(mu3-CNCH2Ph)(mu3-eta1:eta2:eta1-C60) (3) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.893(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.150(2)
_cell_length_b                   26.853(5)
_cell_length_c                   19.273(5)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.00
_cell_measurement_theta_min      1.36
_cell_volume                     6400(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Simens SMART diffractometer/CCD area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7848
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    6.099
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          '0.82x0.23x0.14 mm3'
_refine_diff_density_max         2.429
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         7848
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.330
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0546P)^2^+169.2334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                6954
_reflns_number_total             7848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205703.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/C
_cod_database_code               4077086