The First Structurally Confirmed Paddlewheel Compound with an M27+ Core: [Os2(hpp)4Cl2](PF6)
F. Albert Cotton; Naresh S. Dalal; Penglin Huang; Carlos A. Murillo; Ashley C. Stowe; Xiaoping Wang; Inorganic Chemistry 42 (2003) 670–672; doi:10.1021/ic026250t

data_4313077
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, PO Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 The First Structurally Confirmed Paddlewheel Compound with an M27+ Core:
 [Os2(hpp)4Cl2](PF6)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              670
_journal_page_last               672
_journal_paper_doi               10.1021/ic026250t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '(Os2 N12 C28 H48 Cl2)+, (PF6)-, 2(O1 C3 H6)'
_chemical_formula_sum            'C34 H60 Cl2 F6 N12 O2 Os2 P'
_chemical_formula_weight         1265.21
_chemical_name_common            '[Os2(hpp)4Cl2](PF6) 2acetone'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2820(15)
_cell_length_b                   25.425(2)
_cell_length_c                   10.1454(9)
_cell_measurement_reflns_used    5797
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.46
_cell_volume                     4457.8(7)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V. 5.618'
_computing_data_reduction        'SAINT V. 6.22 and SHELXTL V. 6.10'
_computing_molecular_graphics    'SHELXTL V. 6.10'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27204
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        none
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.922
_exptl_absorpt_correction_T_max  0.3444
_exptl_absorpt_correction_T_min  0.2403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V. 1.03'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5209
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+25.0392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                4318
_reflns_number_total             5209
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic026250t-2_s1_1.cif
_cod_data_source_block           2*2acetone
_cod_original_cell_volume        4457.9(7)
_cod_database_code               4313077