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_4077087
_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)(mu3-CNCH2Ph)(PMe3)(mu3-eta1:eta2:eta1-C60).CS2 (4.CS2)'
_chemical_formula_sum            'C87 H23 N2 O7 Os3 P S2'
_chemical_formula_weight         1873.76
_chemical_name_systematic
; 
 Os3(CO)7(CNCH2Ph)(mu3-CNCH2Ph)(PMe3)(mu3-eta1:eta2:eta1-C60) (4) 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.297(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.685(3)
_cell_length_b                   13.935(3)
_cell_length_c                   29.747(5)
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      1.44
_cell_volume                     5924(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(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  0.2408
_diffrn_reflns_av_sigmaI/netI    0.1584
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24805
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    6.587
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          '0.94x0.18x0.04 mm3'
_refine_diff_density_max         2.638
_refine_diff_density_min         -3.290
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+20.8584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                6180
_reflns_number_total             8251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0205703.cif
_cod_data_source_block           4
_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_cell_volume        5924.1(18)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4077087