Mono- and dinuclear osmium N,N'-di- and tetraphenylbipyridyls and extended bipyridyls. Synthesis, structure and electrochemistry.
Esteruelas, Miguel A.; Fernández, Israel; Gómez-Gallego, Mar; Martín-Ortíz, Mamen; Molina, Pedro; Oliván, Montserrat; Otón, Francisco; Sierra, Miguel A.; Valencia, Marta; Dalton transactions (Cambridge, England : 2003) 42 (2013) 3597–3608; doi:10.1039/c2dt32548a

data_7022413
_publ_section_title
;
 Mono- and dinuclear osmium N,N'-di- and tetraphenylbipyridyls and
 extended bipyridyls. Synthesis, structure and electrochemistry.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3597
_journal_page_last               3608
_journal_paper_doi               10.1039/c2dt32548a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C40 H60 N2 Os P2'
_chemical_formula_weight         821.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.2450(10)
_cell_angle_beta                 76.4900(10)
_cell_angle_gamma                80.7930(10)
_cell_formula_units_Z            2
_cell_length_a                   8.5681(6)
_cell_length_b                   14.7204(10)
_cell_length_c                   15.3568(11)
_cell_measurement_reflns_used    6777
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1841.4(2)
_computing_cell_refinement       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_reduction
;
SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20686
_diffrn_reflns_theta_full        26.62
_diffrn_reflns_theta_max         26.62
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.580
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.111
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7671
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0063P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                6571
_reflns_number_total             7671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32548a.txt
_cod_data_source_block           montse1as
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7022413