Aromatic Diosmatricyclic Nitrogen-Containing Compounds
Miguel A. Esteruelas; Ana B. Masamunt; Montserrat Oliván; Enrique Oñate; Marta Valencia; Journal of the American Chemical Society 130 (2008) 11612–11613; doi:10.1021/ja8048892

data_4108293
_publ_contact_author
;
  Dr. Montserrat Oliv\'an
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 Aromatic Diosmatricyclic Nitrogen-Containing Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11612
_journal_page_last               11613
_journal_paper_doi               10.1021/ja8048892
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C60 H112 N2 Os2 P4, 0.5 (C7 H8)'
_chemical_formula_sum            'C63.5 H116 N2 Os2 P4'
_chemical_formula_weight         1411.86
_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                85.937(8)
_cell_angle_beta                 69.937(8)
_cell_angle_gamma                84.575(7)
_cell_formula_units_Z            2
_cell_length_a                   12.091(5)
_cell_length_b                   16.911(7)
_cell_length_c                   17.257(7)
_cell_measurement_reflns_used    11470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     3297(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.912
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41028
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.94
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.984
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.662
_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 orange'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             1446
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.922
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         15903
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                12342
_reflns_number_total             15903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8048892_si_002_3.cif
_cod_data_source_block           mae328as
_cod_original_formula_sum        'C63.50 H116 N2 Os2 P4'
_cod_database_code               4108293