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_7022414
_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_moiety         'C58 H104 N2 Os2 P4, 2(C7 H8)'
_chemical_formula_sum            'C72 H120 N2 Os2 P4'
_chemical_formula_weight         1517.98
_chemical_name_systematic
;
?
;
_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                 103.864(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.258(4)
_cell_length_b                   8.775(2)
_cell_length_c                   23.919(6)
_cell_measurement_reflns_used    3750
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     3516.7(14)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.940
_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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43143
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.741
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.655
_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 violet'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         8774
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                5956
_reflns_number_total             8774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32548a.txt
_cod_data_source_block           mae389as
_cod_original_cell_volume        3516.5(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7022414