#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/60/2206078.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2206078
loop_
_publ_author_name
'Sun, Bai-Wang'
'Du Lin'
_publ_section_title
;
 Diazidobis(1,7-phenanthroline)zinc(II)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1099
_journal_page_last               m1100
_journal_paper_doi               10.1107/S1600536805014108
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Zn (N3)2 (C12 H8 N2)2]'
_chemical_formula_moiety         'C24 H16 N10 Zn'
_chemical_formula_sum            'C24 H16 N10 Zn'
_chemical_formula_weight         509.84
_chemical_name_systematic
;
Diazidobis(1,7-phenanthroline)zinc(II)
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.7823(13)
_cell_length_b                   17.5908(17)
_cell_length_c                   18.1368(18)
_cell_measurement_reflns_used    18030
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.32
_cell_volume                     4397.1(7)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18030
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0691P)²+1.193P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                2346
_reflns_number_total             3214
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            su6194.cif
_cod_data_source_block           I
_cod_database_code               2206078
_cod_database_fobs_code          2206078
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+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-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+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Zn1 0.2500 0.186831(18) 0.5000 0.03046(13) Uani d S 1 Zn
N1 0.28503(16) 0.24571(13) 0.41260(13) 0.0556(6) Uani d . 1 N
N2 0.22804(14) 0.26275(12) 0.36704(12) 0.0455(5) Uani d . 1 N
N3 0.1759(2) 0.27972(19) 0.32123(16) 0.0891(9) Uani d . 1 N
N4 0.12407(11) 0.12997(9) 0.47862(9) 0.0275(3) Uani d . 1 N
N5 -0.07213(12) -0.04606(10) 0.34128(11) 0.0352(4) Uani d . 1 N
C1 0.20011(13) 0.04145(12) 0.39642(12) 0.0322(4) Uani d . 1 C
H1A 0.2610 0.0624 0.4079 0.039 Uiso calc R 1 H
C2 0.19409(14) -0.01845(12) 0.34947(12) 0.0343(4) Uani d . 1 C
H2A 0.2513 -0.0388 0.3293 0.041 Uiso calc R 1 H
C3 0.09528(16) -0.11401(11) 0.28265(12) 0.0371(5) Uani d . 1 C
H3A 0.1510 -0.1374 0.2632 0.044 Uiso calc R 1 H
C4 0.00450(16) -0.14043(13) 0.26537(12) 0.0403(5) Uani d . 1 C
H4A -0.0032 -0.1820 0.2333 0.048 Uiso calc R 1 H
C5 -0.07613(15) -0.10478(12) 0.29613(13) 0.0407(5) Uani d . 1 C
H5A -0.1377 -0.1239 0.2839 0.049 Uiso calc R 1 H
C6 -0.05925(14) 0.07644(11) 0.44182(12) 0.0321(4) Uani d . 1 C
H6A -0.1216 0.0597 0.4285 0.039 Uiso calc R 1 H
C7 -0.04867(15) 0.13272(13) 0.49300(11) 0.0351(5) Uani d . 1 C
H7A -0.1031 0.1543 0.5161 0.042 Uiso calc R 1 H
C8 0.04435(16) 0.15738(13) 0.51017(11) 0.0330(4) Uani d . 1 C
H8A 0.0513 0.1955 0.5461 0.040 Uiso calc R 1 H
C9 0.11483(13) 0.07261(10) 0.42825(11) 0.0261(4) Uani d . 1 C
C10 0.10300(14) -0.05116(10) 0.33011(11) 0.0299(4) Uani d . 1 C
C11 0.01741(13) -0.01922(10) 0.35832(11) 0.0273(4) Uani d . 1 C
C12 0.02268(13) 0.04355(10) 0.40913(11) 0.0263(4) Uani d . 1 C
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'
Zn Zn 0.2839 1.4301 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Zn1 N1 7_545 . 115.98(15) y
N1 Zn1 N4 7_545 . 101.76(8) y
N1 Zn1 N4 . . 108.41(8) y
N1 Zn1 N4 7_545 7_545 108.41(8) ?
N1 Zn1 N4 . 7_545 101.76(8) ?
N4 Zn1 N4 . 7_545 121.29(9) y
N2 N1 Zn1 . . 122.60(18) y
N3 N2 N1 . . 177.4(3) y
C8 N4 C9 . . 118.58(17) y
C8 N4 Zn1 . . 116.33(13) y
C9 N4 Zn1 . . 124.61(13) y
C5 N5 C11 . . 116.86(18) ?
C2 C1 C9 . . 120.28(17) ?
C2 C1 H1A . . 119.9 ?
C9 C1 H1A . . 119.9 ?
C1 C2 C10 . . 121.46(18) ?
C1 C2 H2A . . 119.3 ?
C10 C2 H2A . . 119.3 ?
C4 C3 C10 . . 118.4(2) ?
C4 C3 H3A . . 120.8 ?
C10 C3 H3A . . 120.8 ?
C3 C4 C5 . . 118.9(2) ?
C3 C4 H4A . . 120.5 ?
C5 C4 H4A . . 120.5 ?
N5 C5 C4 . . 124.61(19) ?
N5 C5 H5A . . 117.7 ?
C4 C5 H5A . . 117.7 ?
C7 C6 C12 . . 120.10(18) ?
C7 C6 H6A . . 119.9 ?
C12 C6 H6A . . 119.9 ?
C6 C7 C8 . . 118.53(19) ?
C6 C7 H7A . . 120.7 ?
C8 C7 H7A . . 120.7 ?
N4 C8 C7 . . 123.58(19) ?
N4 C8 H8A . . 118.2 ?
C7 C8 H8A . . 118.2 ?
N4 C9 C12 . . 120.99(17) ?
N4 C9 C1 . . 118.66(16) ?
C12 C9 C1 . . 120.33(17) ?
C11 C10 C3 . . 118.34(17) ?
C11 C10 C2 . . 119.29(17) ?
C3 C10 C2 . . 122.36(19) ?
N5 C11 C10 . . 122.83(17) ?
N5 C11 C12 . . 117.29(17) ?
C10 C11 C12 . . 119.86(16) ?
C6 C12 C9 . . 118.14(17) ?
C6 C12 C11 . . 123.17(17) ?
C9 C12 C11 . . 118.69(17) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N1 7_545 1.954(2) y
Zn1 N1 . 1.954(2) ?
Zn1 N4 . 2.0403(16) y
Zn1 N4 7_545 2.0403(16) ?
N1 N2 . 1.179(3) y
N2 N3 . 1.138(3) y
N4 C8 . 1.329(3) y
N4 C9 . 1.367(2) y
N5 C5 . 1.319(3) y
N5 C11 . 1.357(2) y
C1 C2 . 1.357(3) ?
C1 C9 . 1.420(3) ?
C1 H1A . 0.9400 ?
C2 C10 . 1.425(3) ?
C2 H2A . 0.9400 ?
C3 C4 . 1.371(3) ?
C3 C10 . 1.405(3) ?
C3 H3A . 0.9400 ?
C4 C5 . 1.393(3) ?
C4 H4A . 0.9400 ?
C5 H5A . 0.9400 ?
C6 C7 . 1.365(3) ?
C6 C12 . 1.400(3) ?
C6 H6A . 0.9400 ?
C7 C8 . 1.389(3) ?
C7 H7A . 0.9400 ?
C8 H8A . 0.9400 ?
C9 C12 . 1.412(2) ?
C10 C11 . 1.403(3) ?
C11 C12 . 1.440(3) ?
