#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:49:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179395 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329253.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_4329253
loop_
_publ_author_name
'Benjamin Lyhs'
'Dieter Bläser'
'Christoph Wölper'
'Stephan Schulz'
'Georg Jansen'
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen, Universitätsstr. 7
         D-45141 Essen, Germany
;
_publ_contact_author_email       stephan.schulz@.uni-due.de
_publ_contact_author_fax         '++49 (0)201 183 3830'
_publ_contact_author_phone       '++49 (0)201 183 4635'
_publ_section_title
;
 First Structural Characterization of Neutral, Base-Stabilized Group
 15-Pentaazides: Single Crystal X-ray Structures of dmap-As(N3)5 and
 dmap-Sb(N3)5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5902
_journal_paper_doi               10.1021/ic300523k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C7 H10 As N17'
_chemical_formula_sum            'C7 H10 As N17'
_chemical_formula_weight         407.24
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.9789(5)
_cell_length_b                   7.8016(2)
_cell_length_c                   22.2904(6)
_cell_measurement_reflns_used    41357
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.15
_cell_volume                     3126.54(15)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            86329
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0273
_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/[σ²(Fo²)+(0.0200P)²+2.7773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                4009
_reflns_number_total             4732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300523k_si_002_1.cif
_cod_data_source_block           ben_137m
_cod_database_code               4329253
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
As1 As 0.093030(8) 0.024135(19) 0.356648(6) 0.01116(4) Uani 1 1 d .
N1 N 0.13816(7) 0.24156(17) 0.37478(6) 0.0160(2) Uani 1 1 d .
N2 N 0.09420(7) 0.34520(16) 0.39694(6) 0.0147(2) Uani 1 1 d .
N3 N 0.05737(8) 0.44701(18) 0.41749(7) 0.0211(3) Uani 1 1 d .
N4 N 0.04826(7) -0.19416(16) 0.33799(6) 0.0157(2) Uani 1 1 d .
N5 N 0.08784(7) -0.29840(17) 0.31173(6) 0.0160(2) Uani 1 1 d .
N6 N 0.11985(8) -0.40177(19) 0.28706(7) 0.0247(3) Uani 1 1 d .
N7 N 0.05590(8) 0.00960(17) 0.43796(6) 0.0179(3) Uani 1 1 d .
N8 N 0.07449(7) -0.11722(17) 0.46702(6) 0.0148(2) Uani 1 1 d .
N9 N 0.08921(9) -0.2282(2) 0.49733(7) 0.0271(3) Uani 1 1 d .
N10 N 0.18641(7) -0.09005(18) 0.37085(6) 0.0161(3) Uani 1 1 d .
N11 N 0.22454(7) -0.03129(18) 0.41154(6) 0.0175(3) Uani 1 1 d .
N12 N 0.26273(9) 0.0147(2) 0.44849(7) 0.0307(4) Uani 1 1 d .
N13 N 0.00330(7) 0.13903(16) 0.33228(6) 0.0146(2) Uani 1 1 d .
N14 N -0.05505(7) 0.07653(17) 0.35103(6) 0.0154(2) Uani 1 1 d .
N15 N -0.11120(8) 0.0277(2) 0.36571(8) 0.0271(3) Uani 1 1 d .
N16 N 0.12610(7) 0.05353(16) 0.27233(6) 0.0131(2) Uani 1 1 d .
N17 N 0.17629(7) 0.18426(17) 0.09668(6) 0.0146(2) Uani 1 1 d .
C1 C 0.19173(8) 0.1306(2) 0.25881(7) 0.0159(3) Uani 1 1 d .
H1 H 0.2252 0.1571 0.2905 0.019 Uiso 1 1 d R
C2 C 0.21143(8) 0.1713(2) 0.20156(7) 0.0162(3) Uani 1 1 d .
H2 H 0.2582 0.2235 0.1940 0.019 Uiso 1 1 d R
C3 C 0.16238(8) 0.13619(19) 0.15318(6) 0.0131(3) Uani 1 1 d .
C4 C 0.09649(8) 0.04543(19) 0.16808(7) 0.0140(3) Uani 1 1 d .
H4 H 0.0635 0.0098 0.1372 0.017 Uiso 1 1 d R
C5 C 0.08027(8) 0.00923(19) 0.22637(7) 0.0138(3) Uani 1 1 d .
H5 H 0.0353 -0.0492 0.2353 0.017 Uiso 1 1 d R
C6 C 0.24354(9) 0.2775(2) 0.08047(7) 0.0196(3) Uani 1 1 d .
H6A H 0.2373 0.3991 0.0903 0.029 Uiso 1 1 d R
H6B H 0.2527 0.2651 0.0373 0.029 Uiso 1 1 d R
H6C H 0.2859 0.2309 0.1029 0.029 Uiso 1 1 d R
C7 C 0.11900(9) 0.1662(2) 0.05031(7) 0.0193(3) Uani 1 1 d .
H7A H 0.1136 0.0450 0.0396 0.029 Uiso 1 1 d R
H7B H 0.1335 0.2318 0.0147 0.029 Uiso 1 1 d R
H7C H 0.0715 0.2097 0.0656 0.029 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 As1 N13 90.12(5)
N1 As1 N10 90.32(6)
N13 As1 N10 172.97(5)
N1 As1 N4 179.59(6)
N13 As1 N4 90.03(5)
N10 As1 N4 89.48(6)
N1 As1 N7 90.02(6)
N13 As1 N7 90.14(6)
N10 As1 N7 96.87(6)
N4 As1 N7 90.36(6)
N1 As1 N16 88.33(6)
N13 As1 N16 85.98(5)
N10 As1 N16 87.02(5)
N4 As1 N16 91.31(5)
N7 As1 N16 175.78(5)
N2 N1 As1 113.07(10)
N3 N2 N1 175.85(15)
N5 N4 As1 116.44(10)
N6 N5 N4 174.98(16)
N8 N7 As1 116.56(10)
N9 N8 N7 174.89(16)
N11 N10 As1 115.84(10)
N12 N11 N10 175.70(16)
N14 N13 As1 115.76(10)
N15 N14 N13 174.97(16)
C1 N16 C5 118.16(13)
C1 N16 As1 121.43(10)
C5 N16 As1 120.19(10)
C3 N17 C6 121.92(13)
C3 N17 C7 120.37(13)
C6 N17 C7 117.15(12)
N16 C1 C2 122.47(14)
C1 C2 C3 120.35(13)
N17 C3 C4 121.07(13)
N17 C3 C2 123.03(13)
C4 C3 C2 115.90(13)
C5 C4 C3 120.37(13)
N16 C5 C4 122.46(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
As1 N1 1.9233(13)
As1 N13 1.9238(12)
As1 N10 1.9268(13)
As1 N4 1.9291(13)
As1 N7 1.9348(13)
As1 N16 1.9846(12)
N1 N2 1.2338(18)
N2 N3 1.1310(19)
N4 N5 1.2290(18)
N5 N6 1.1331(19)
N7 N8 1.2290(18)
N8 N9 1.1297(19)
N10 N11 1.2258(18)
N11 N12 1.131(2)
N13 N14 1.2302(17)
N14 N15 1.1273(19)
N16 C1 1.3584(18)
N16 C5 1.3593(19)
N17 C3 1.3377(18)
N17 C6 1.4564(19)
N17 C7 1.466(2)
C1 C2 1.362(2)
C2 C3 1.420(2)
C3 C4 1.420(2)
C4 C5 1.361(2)
