#------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/00/4020090.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4020090
loop_
_publ_author_name
'Unciti-Broceta, A.'
'Pineda-de-las-Infantas, M.J.'
'Díaz-Mochón, J.J.'
'Romagnoli, R.'
'Baraldi, P.G.'
'Gallo, M.A.'
'Espinosa, A.'
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2878
_journal_page_last               2880
_journal_paper_doi               10.1021/jo0478398
_journal_volume                  70
_journal_year                    2005
_chemical_formula_sum            'C15 H13 N7'
_chemical_formula_weight         291.31
_chemical_name_systematic
;
 6,11-dicyclopropylpyrido[2,3-e]Bis[1,2,4]triazolo[4,3-a:3',4'-c]pyrazine
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.2462(6)
_cell_length_b                   8.8456(6)
_cell_length_c                   32.222(2)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     2635.3(3)
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            15327
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.09
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+0.9789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                2454
_reflns_number_total             3073
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4020090
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.57478(15) 0.13858(16) 0.33783(5) 0.0369(3) Uani 1 1 d . . .
N2 N 0.60665(15) -0.05592(17) 0.40434(4) 0.0382(4) Uani 1 1 d . . .
C3 C 0.44900(18) 0.0848(2) 0.35829(5) 0.0363(4) Uani 1 1 d . . .
N4 N 0.81014(17) 0.1791(2) 0.33114(5) 0.0481(4) Uani 1 1 d . . .
C5 C 0.71153(18) 0.1080(2) 0.35238(6) 0.0389(4) Uani 1 1 d . . .
C6 C 0.46512(18) -0.0144(2) 0.39182(6) 0.0373(4) Uani 1 1 d . . .
N7 N 0.84597(17) -0.0564(2) 0.40108(5) 0.0499(4) Uani 1 1 d . . .
C8 C 0.72852(18) 0.0019(2) 0.38563(6) 0.0395(4) Uani 1 1 d . . .
C9 C 0.2185(2) -0.0272(3) 0.40010(7) 0.0527(5) Uani 1 1 d . . .
N10 N 0.73664(18) 0.2563(2) 0.30015(5) 0.0512(4) Uani 1 1 d . . .
N11 N 0.35202(18) -0.0705(2) 0.41264(5) 0.0509(4) Uani 1 1 d . . .
N12 N 0.80111(18) -0.1575(2) 0.43154(6) 0.0530(5) Uani 1 1 d . . .
C13 C 0.1974(2) 0.0714(3) 0.36807(7) 0.0537(5) Uani 1 1 d . . .
C14 C 0.5980(2) 0.2316(2) 0.30414(6) 0.0422(4) Uani 1 1 d . . .
C15 C 0.6601(2) -0.1566(2) 0.43349(6) 0.0451(5) Uani 1 1 d . . .
C16 C 0.3138(2) 0.1279(3) 0.34717(7) 0.0458(5) Uani 1 1 d . . .
C17 C 0.4887(2) 0.2894(2) 0.27515(6) 0.0457(5) Uani 1 1 d . . .
C18 C 0.5410(3) 0.3748(3) 0.23806(8) 0.0623(6) Uani 1 1 d . . .
C19 C 0.5759(3) -0.2437(3) 0.46358(7) 0.0571(6) Uani 1 1 d . . .
C20 C 0.4637(3) 0.4563(3) 0.27139(9) 0.0634(7) Uani 1 1 d . . .
C21 C 0.6537(4) -0.3442(4) 0.49274(9) 0.0739(8) Uani 1 1 d . . .
C22 C 0.5896(4) -0.2055(4) 0.50839(9) 0.0785(8) Uani 1 1 d . . .
H1 H 0.411(2) 0.225(2) 0.2708(7) 0.057(6) Uiso 1 1 d . . .
H2 H 0.307(2) 0.180(2) 0.3314(7) 0.041(7) Uiso 1 1 d . . .
H3 H 0.105(3) 0.104(3) 0.3606(7) 0.066(7) Uiso 1 1 d . . .
H4 H 0.519(3) 0.515(3) 0.2891(9) 0.084(9) Uiso 1 1 d . . .
H5 H 0.482(3) 0.351(3) 0.2128(9) 0.075(7) Uiso 1 1 d . . .
H6 H 0.139(3) -0.069(3) 0.4144(7) 0.067(7) Uiso 1 1 d . . .
H7 H 0.487(3) -0.275(3) 0.4550(8) 0.069(7) Uiso 1 1 d . . .
H8 H 0.361(3) 0.485(3) 0.2673(8) 0.074(8) Uiso 1 1 d . . .
H9 H 0.647(3) 0.393(3) 0.2361(8) 0.081(8) Uiso 1 1 d . . .
H10 H 0.604(3) -0.440(4) 0.5009(9) 0.101(10) Uiso 1 1 d . . .
H11 H 0.757(4) -0.346(3) 0.4910(9) 0.098(10) Uiso 1 1 d . . .
H12 H 0.658(3) -0.128(3) 0.5141(9) 0.092(9) Uiso 1 1 d . . .
H13 H 0.513(4) -0.215(4) 0.5244(11) 0.109(11) Uiso 1 1 d . . .
