#------------------------------------------------------------------------------
#$Date: 2017-05-05 08:49:52 +0300 (Fri, 05 May 2017) $
#$Revision: 196234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012424.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_2012424
loop_
_publ_author_name
'Cheng, Ya-Qian'
'Hu, Mao-Lin'
'Wang, Shun'
'Ye, Ming-De'
_publ_section_title
;
 μ~1,3~-Azido-diazidotetrakis(1,10-phenanthroline)dicopper(II) azide
 tetrahydrate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m12
_journal_page_last               m13
_journal_paper_doi               10.1107/S0108270101016948
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Cu(C12H8N2)2(N3)],N3,2H2O'
_chemical_formula_moiety         'C24 H16 Cu N7,N3,2(H2O)'
_chemical_formula_sum            'C24 H20 Cu N10 O2'
_chemical_formula_weight         544.04
_chemical_name_systematic
;
Diazido μ~1,3~-azidotetra(1,10-phenanthroline)
diCopper(II) azide tetrahydrate
;
_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                80.810(10)
_cell_angle_beta                 71.740(10)
_cell_angle_gamma                84.600(10)
_cell_formula_units_Z            2
_cell_length_a                   8.676(5)
_cell_length_b                   11.843(8)
_cell_length_c                   12.279(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      1.47
_cell_volume                     1181.4(13)
_computing_cell_refinement       SMART1000
_computing_data_collection       'SMART1000 (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1998)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .988
_diffrn_measured_fraction_theta_max .988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0213
_diffrn_reflns_av_sigmaI/netI    .0488
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6191
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        none
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    .970
_exptl_absorpt_correction_T_max  .890
_exptl_absorpt_correction_T_min  .858
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             558
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .12
_refine_diff_density_max         .366
_refine_diff_density_min         -.429
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          .0650
_refine_ls_R_factor_gt           .0458
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0587P)²+0.7136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1078
_refine_ls_wR_factor_ref         .1209
_reflns_number_gt                3239
_reflns_number_total             4133
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            de1175.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.7136P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.7136P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2017-04-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H40 Cu2 N20 O4'
_cod_original_formula_weight         1088.08
_cod_original_formula_moiety         'C48 H32 Cu2 N17,N3,4(H2O)'
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012424
_cod_database_fobs_code          2012424
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu1 .12897(5) .26244(4) .36525(3) .04023(16) Uani d . 1 . . Cu
N1 .0460(4) .0373(3) .4007(4) .0671(10) Uani d . 1 . . N
N2 .0000 .0000 .5000 .0552(12) Uani d S 1 . . N
N3 -.1025(4) .3100(3) .4176(3) .0519(8) Uani d . 1 . . N
N4 -.1658(4) .3764(3) .3619(3) .0631(9) Uani d . 1 . . N
N5 -.2339(7) .4393(6) .3104(4) .143(3) Uani d . 1 . . N
N6 .1401(3) .2288(2) .5283(2) .0378(6) Uani d . 1 . . N
N7 .3610(3) .1903(2) .3309(2) .0373(6) Uani d . 1 . . N
N8 .2513(4) .4353(3) .3252(2) .0444(7) Uani d . 1 . . N
N9 .1444(3) .3108(3) .1971(2) .0414(7) Uani d . 1 . . N
N10 .1188(7) -.0298(6) .0179(4) .122(2) Uani d . 1 . . N
N11 .0000 .0000 .0000 .0647(13) Uani d S 1 . . N
C1 .0247(4) .2452(3) .6260(3) .0485(9) Uani d . 1 . . C
H1A -.0821 .2713 .6225 .080 Uiso d R 1 . . H
C2 .0546(5) .2263(4) .7328(3) .0570(10) Uani d . 1 . . C
H2A -.0317 .2387 .8019 .080 Uiso d R 1 . . H
C3 .2056(5) .1903(4) .7385(3) .0540(10) Uani d . 1 . . C
H3A .2275 .1768 .8115 .080 Uiso d R 1 . . H
C4 .3316(4) .1724(3) .6369(3) .0410(8) Uani d . 1 . . C
C5 .2910(4) .1926(3) .5339(3) .0346(7) Uani d . 1 . . C
C6 .4114(4) .1739(3) .4268(3) .0362(7) Uani d . 1 . . C
C7 .5701(4) .1392(3) .4262(3) .0417(8) Uani d . 1 . . C
C8 .6827(4) .1209(3) .3181(3) .0511(9) Uani d . 1 . . C
H8A .7940 .0989 .3124 .080 Uiso d R 1 . . H
C9 .6312(5) .1356(3) .2223(4) .0568(10) Uani d . 1 . . C
H9A .7068 .1222 .1490 .080 Uiso d R 1 . . H
C10 .4690(4) .1699(3) .2317(3) .0478(9) Uani d . 1 . . C
H10A .4347 .1794 .1635 .080 Uiso d R 1 . . H
C11 .6092(4) .1214(3) .5328(4) .0500(9) Uani d . 1 . . C
H11A .7185 .0980 .5321 .080 Uiso d R 1 . . H
C12 .4942(5) .1366(3) .6333(3) .0486(9) Uani d . 1 . . C
H12A .5231 .1235 .7038 .080 Uiso d R 1 . . H
C13 .3111(5) .4915(3) .3864(4) .0535(10) Uani d . 1 . . C
H13A .2973 .4614 .4661 .080 Uiso d R 1 . . H
C14 .3920(5) .5926(4) .3411(4) .0611(11) Uani d . 1 . . C
H14A .4371 .6297 .3874 .080 Uiso d R 1 . . H
C15 .4093(5) .6377(4) .2294(4) .0635(11) Uani d . 1 . . C
H15A .4631 .7082 .1976 .080 Uiso d R 1 . . H
C16 .3453(4) .5814(3) .1606(3) .0509(9) Uani d . 1 . . C
C17 .2696(4) .4784(3) .2130(3) .0411(8) Uani d . 1 . . C
C18 .2102(4) .4137(3) .1462(3) .0414(8) Uani d . 1 . . C
C19 .2197(4) .4579(3) .0306(3) .0500(9) Uani d . 1 . . C
C20 .1561(5) .3930(4) -.0302(3) .0604(11) Uani d . 1 . . C
H20A .1618 .4198 -.1094 .080 Uiso d R 1 . . H
C21 .0873(5) .2920(4) .0232(3) .0581(11) Uani d . 1 . . C
H21A .0408 .2481 -.0170 .080 Uiso d R 1 . . H
C22 .0854(4) .2528(4) .1366(3) .0487(9) Uani d . 1 . . C
H22A .0384 .1809 .1731 .080 Uiso d R 1 . . H
C23 .2941(5) .5659(4) -.0181(4) .0649(12) Uani d . 1 . . C
H23A .3033 .5950 -.0974 .080 Uiso d R 1 . . H
C24 .3527(5) .6238(4) .0438(4) .0638(12) Uani d . 1 . . C
H24A .3996 .6962 .0095 .080 Uiso d R 1 . . H
O1W .2627(4) -.0484(4) .1944(3) .0935(11) Uani d . 1 . . O
H1WA .2658 .0061 .1292 .080 Uiso d R 1 . . H
H1WB .2623 -.0157 .2594 .080 Uiso d R 1 . . H
O2W .5689(4) -.1273(3) .0509(3) .0857(10) Uani d . 1 . . O
H2WA .6443 -.0694 .0268 .080 Uiso d R 1 . . H
H2WB .4693 -.1006 .0989 .080 Uiso d R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu .3201 1.2651 '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
N3 Cu1 N6 . . 92.21(12) yes
N3 Cu1 N9 . . 92.55(12) yes
N6 Cu1 N9 . . 171.83(11) yes
N3 Cu1 N7 . . 170.71(12) yes
N6 Cu1 N7 . . 81.49(11) yes
N9 Cu1 N7 . . 94.53(11) yes
N3 Cu1 N8 . . 101.94(13) yes
N6 Cu1 N8 . . 94.74(11) yes
N9 Cu1 N8 . . 77.76(11) yes
N7 Cu1 N8 . . 85.46(11) yes
N3 Cu1 N1 . . 89.61(13) yes
N6 Cu1 N1 . . 84.32(12) yes
N9 Cu1 N1 . . 102.36(12) yes
N7 Cu1 N1 . . 83.02(11) yes
N8 Cu1 N1 . . 168.45(11) yes
N2 N1 Cu1 . . 112.5(2) yes
N2 N1 O1W . . 134.6(3) no
Cu1 N1 O1W . . 102.11(16) no
N1 N2 N1 2_556 . 180.0 no
N4 N3 Cu1 . . 123.4(3) yes
N5 N4 N3 . . 177.0(5) no
C1 N6 C5 . . 118.3(3) no
C1 N6 Cu1 . . 128.5(2) no
C5 N6 Cu1 . . 113.0(2) no
C10 N7 C6 . . 117.5(3) no
C10 N7 Cu1 . . 130.7(2) no
C6 N7 Cu1 . . 111.3(2) no
C13 N8 C17 . . 118.3(3) no
C13 N8 Cu1 . . 132.9(3) no
C17 N8 Cu1 . . 108.6(2) no
C22 N9 C18 . . 118.7(3) no
C22 N9 Cu1 . . 124.0(3) no
C18 N9 Cu1 . . 117.1(2) no
N11 N10 O1W . . 140.3(4) no
N10 N11 N10 2 . 180.0 no
N6 C1 C2 . . 121.9(3) no
C3 C2 C1 . . 119.7(4) no
C2 C3 C4 . . 120.2(3) no
C5 C4 C3 . . 116.4(3) no
C5 C4 C12 . . 119.1(3) no
C3 C4 C12 . . 124.5(3) no
N6 C5 C4 . . 123.5(3) no
N6 C5 C6 . . 116.6(3) no
C4 C5 C6 . . 120.0(3) no
N7 C6 C7 . . 124.0(3) no
N7 C6 C5 . . 116.6(3) no
C7 C6 C5 . . 119.4(3) no
C6 C7 C8 . . 116.7(3) no
C6 C7 C11 . . 119.4(3) no
C8 C7 C11 . . 123.8(3) no
C9 C8 C7 . . 119.2(3) no
C8 C9 C10 . . 119.9(4) no
C8 C9 N10 . 2_655 117.3(3) no
C10 C9 N10 . 2_655 121.4(3) no
N7 C10 C9 . . 122.6(4) no
C12 C11 C7 . . 120.6(3) no
C11 C12 C4 . . 121.4(3) no
N8 C13 C14 . . 123.1(4) no
C15 C14 C13 . . 119.3(4) no
C14 C15 C16 . . 119.7(4) no
C17 C16 C15 . . 116.9(4) no
C17 C16 C24 . . 119.2(4) no
C15 C16 C24 . . 123.9(4) no
N8 C17 C16 . . 122.7(3) no
N8 C17 C18 . . 117.7(3) no
C16 C17 C18 . . 119.7(3) no
N9 C18 C19 . . 121.6(3) no
N9 C18 C17 . . 118.8(3) no
C19 C18 C17 . . 119.6(3) no
C20 C19 C18 . . 117.6(4) no
C20 C19 C23 . . 124.0(4) no
C18 C19 C23 . . 118.5(4) no
C21 C20 C19 . . 119.9(4) no
C20 C21 C22 . . 119.3(4) no
N9 C22 C21 . . 122.9(4) no
C24 C23 C19 . . 121.4(4) no
C23 C24 C16 . . 121.5(4) no
N10 O1W O2W . . 92.79(17) yes
N10 O1W N1 . . 112.09(18) yes
O2W O1W N1 . . 154.61(17) yes
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
Cu1 N3 . 1.964(3) yes
Cu1 N6 . 2.009(3) yes
Cu1 N9 . 2.018(3) yes
Cu1 N7 . 2.054(3) yes
Cu1 N8 . 2.306(3) yes
Cu1 N1 . 2.759(4) yes
N1 N2 . 1.182(4) no
N1 O1W . 2.908(5) yes
N2 N1 2_556 1.182(4) no
N3 N4 . 1.171(4) no
N4 N5 . 1.142(5) no
N6 C1 . 1.329(4) no
N6 C5 . 1.358(4) no
N7 C10 . 1.325(4) no
N7 C6 . 1.360(4) no
N8 C13 . 1.321(5) no
N8 C17 . 1.355(4) no
N9 C22 . 1.325(5) no
N9 C18 . 1.366(5) no
N10 N11 . 1.133(6) no
N10 O1W . 2.792(6) no
N11 N10 2 1.133(6) no
C1 C2 . 1.396(5) no
C2 C3 . 1.358(6) no
C3 C4 . 1.408(5) no
C4 C5 . 1.396(5) no
C4 C12 . 1.424(5) no
C5 C6 . 1.435(5) no
C6 C7 . 1.397(5) no
C7 C8 . 1.416(5) no
C7 C11 . 1.431(5) no
C8 C9 . 1.365(6) no
C9 C10 . 1.402(5) no
C9 N10 2_655 3.411(7) no
C11 C12 . 1.348(5) no
C13 C14 . 1.392(6) no
C14 C15 . 1.358(6) no
C15 C16 . 1.417(6) no
C16 C17 . 1.403(5) no
C16 C24 . 1.426(6) no
C17 C18 . 1.437(5) no
C18 C19 . 1.412(5) no
C19 C20 . 1.405(6) no
C19 C23 . 1.442(6) no
C20 C21 . 1.363(6) no
C21 C22 . 1.391(5) no
C23 C24 . 1.335(6) no
O1W O2W . 2.857(5) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WA N10 . .94 2.25 2.792(6) 116.1
O1W H1WB N1 . .94 2.24 2.908(5) 127.5
O2W H2WB O1W . .94 1.92 2.857(5) 178.2
C9 H9A N10 2_655 .94 2.50 3.411(7) 163.4
