#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/97/2019710.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_2019710
loop_
_publ_author_name
'Liu, Hou-Ting'
'Lu, Jing'
_publ_section_title
;
 An azide-bridged copper(II) complex: poly[piperazine-1,4-dium
 [tetra-μ₃-azido-κ¹²N¹:N¹:N¹-hexa-μ₂-azido-κ¹²N¹:N¹-di-μ₂-azido-κ⁴N¹:N³-pentacopper(II)]
 tetrahydrate]
;
_journal_coeditor_code           WQ3076
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1083
_journal_page_last               1087
_journal_paper_doi               10.1107/S2053229614022190
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C4 H12 N2) [Cu5 (N3)12] , 4H2 O'
_chemical_formula_moiety         'C4 H12 N2 2+, Cu5 N36 2-, 4(H2 O)'
_chemical_formula_sum            'C4 H20 Cu5 N38 O4'
_chemical_formula_weight         982.28
_chemical_name_systematic
;Poly[piperazine-1,4-dium
[tetra-μ₃-azido-κ¹²N¹:N¹:N¹-hexa-μ₂-azido-κ¹²N¹:N¹-di-μ₂-azido-κ⁴N¹:N³-pentacopper(II)] tetrahydrate]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.343(3)
_cell_length_b                   5.7477(11)
_cell_length_c                   16.812(3)
_cell_measurement_reflns_used    2772
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.72
_cell_volume                     1578.9(5)
_computing_cell_refinement
;
SMART (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7506
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    3.399
_exptl_absorpt_correction_T_max  0.5644
_exptl_absorpt_correction_T_min  0.5218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.495
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0265P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                2080
_reflns_number_total             2772
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wq3076sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019710.cif.'
_cod_original_cell_volume        1579.0(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019710
_cod_database_fobs_code          2019710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.0000 1.0000 0.5000 0.02402(17) Uani d SU 1 2 . .
Cu Cu2 0.07589(2) 0.57208(8) 0.58419(2) 0.02086(13) Uani d U 1 1 . .
Cu Cu3 0.13723(2) 0.11424(7) 0.66215(2) 0.02121(14) Uani d U 1 1 . .
N N1 0.00263(17) 1.1650(5) 0.39549(16) 0.0245(7) Uani d U 1 1 . .
N N2 0.04243(19) 1.1250(6) 0.33707(19) 0.0325(8) Uani d U 1 1 . .
N N3 0.0785(2) 1.0904(8) 0.2810(2) 0.0705(14) Uani d U 1 1 . .
N N4 0.06828(18) 0.7236(5) 0.47703(16) 0.0265(7) Uani d U 1 1 . .
N N7 0.12900(17) 0.2692(5) 0.55257(16) 0.0226(7) Uani d U 1 1 . .
N N8 0.1836(2) 0.2482(6) 0.50541(19) 0.0333(8) Uani d U 1 1 B .
N N9 0.2340(3) 0.2218(8) 0.4603(2) 0.0767(14) Uani d U 1 1 . .
N N10 0.06509(18) 0.3886(5) 0.68196(17) 0.0273(7) Uani d U 1 1 . .
N N11 0.04725(18) 0.4540(5) 0.74812(19) 0.0272(7) Uani d U 1 1 B .
N N12 0.0300(2) 0.5116(7) 0.8105(2) 0.0518(11) Uani d U 1 1 . .
N N13 0.18198(18) -0.1853(5) 0.62292(17) 0.0276(7) Uani d U 1 1 . .
N N14 0.2487(2) -0.1951(5) 0.59446(17) 0.0280(7) Uani d U 1 1 B .
N N15 0.3128(2) -0.2094(7) 0.5675(2) 0.0534(11) Uani d U 1 1 . .
N N16 0.2715(2) 0.2613(6) 0.6757(2) 0.0471(10) Uani d U 1 1 . .
N N17 0.32242(18) 0.3779(5) 0.70271(17) 0.0273(7) Uani d U 1 1 B .
N N18 0.37683(18) 0.4982(5) 0.72859(17) 0.0303(8) Uani d U 1 1 . .
N N19 0.00763(19) -0.0287(6) 0.91541(17) 0.0382(9) Uani d U 1 1 . .
H H1A 0.0341 0.0032 0.8702 0.046 Uiso calc R 1 1 . .
H H1B -0.0347 -0.1230 0.9032 0.046 Uiso calc R 1 1 . .
C C1 -0.0234(2) 0.1897(7) 0.9499(2) 0.0402(11) Uani d U 1 1 . .
H H19A -0.0624 0.2602 0.9130 0.048 Uiso calc R 1 1 . .
H H19B 0.0217 0.2975 0.9577 0.048 Uiso calc R 1 1 . .
C C2 0.0641(2) -0.1485(7) 0.9720(2) 0.0347(10) Uani d U 1 1 . .
H H2A 0.1127 -0.0543 0.9805 0.042 Uiso calc R 1 1 . .
H H2B 0.0808 -0.2962 0.9496 0.042 Uiso calc R 1 1 . .
O O2 0.87024(18) 0.7007(6) 0.90155(18) 0.0768(11) Uani d U 1 1 . .
H H2E 0.8479 0.6958 0.9468 0.092 Uiso d R 1 1 . .
H H2F 0.8362 0.6508 0.8667 0.092 Uiso d R 1 1 . .
O O1 0.7768(5) 0.545(2) 0.7752(5) 0.108(4) Uani d PU 0.589(11) 1 A 1
H H1E 0.7343 0.6188 0.7886 0.130 Uiso d PR 0.589(11) 1 A 1
H H1F 0.7714 0.5025 0.7269 0.130 Uiso d PR 0.589(11) 1 A 1
O O1' 0.8184(9) 0.363(3) 0.8038(7) 0.126(5) Uani d PU 0.411(11) 1 A 2
H H1'A 0.7716 0.3014 0.8092 0.152 Uiso d PR 0.411(11) 1 A 2
H H1'B 0.8272 0.3799 0.7544 0.152 Uiso d PR 0.411(11) 1 A 2
N N5 0.1105(2) 0.6869(6) 0.4225(2) 0.0365(8) Uani d U 1 1 B 2
N N6 0.1731(14) 0.702(4) 0.3866(15) 0.044(4) Uani d PU 0.29(3) 1 C 1
N N6' 0.1405(10) 0.626(2) 0.3625(6) 0.061(3) Uani d PU 0.71(3) 1 B 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 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
N4 Cu1 N4 . 3_576 180.0000(10) y
N4 Cu1 N1 . . 100.79(11) y
N4 Cu1 N1 3_576 . 79.21(11) y
N4 Cu1 N1 . 3_576 79.21(11) ?
N4 Cu1 N1 3_576 3_576 100.79(11) ?
N1 Cu1 N1 . 3_576 180.0000(10) ?
N1 Cu1 N7 . 1_565 89.22(10) y
N4 Cu1 N7 . 1_565 94.74(10) y
N1 Cu1 N7 3_576 1_565 90.79(10) y
N4 Cu1 N7 3_576 1_565 85.26(10) y
N10 Cu2 N4 . . 168.95(13) y
N10 Cu2 N1 . 3_576 101.13(12) y
N4 Cu2 N1 . 3_576 78.33(11) y
N10 Cu2 N7 . . 78.67(12) y
N4 Cu2 N7 . . 99.06(11) y
N1 Cu2 N7 3_576 . 165.54(12) y
N10 Cu2 N13 . 1_565 99.63(12) y
N4 Cu2 N13 . 1_565 91.40(12) y
N1 Cu2 N13 3_576 1_565 88.66(12) y
N7 Cu2 N13 . 1_565 105.68(11) y
N18 Cu3 N13 2_546 . 93.81(13) y
N18 Cu3 N10 2_546 . 91.83(12) y
N13 Cu3 N10 . . 163.64(12) y
N18 Cu3 N7 2_546 . 167.98(12) y
N13 Cu3 N7 . . 95.54(12) y
N10 Cu3 N7 . . 77.18(11) y
N18 Cu3 N16 2_546 . 98.96(13) y
N13 Cu3 N16 . . 89.72(12) y
N10 Cu3 N16 . . 104.56(13) y
N7 Cu3 N16 . . 88.64(12) y
N7 Cu3 N1 . 3_566 85.48(10) y
N13 Cu3 N1 . 3_566 72.94(10) y
N10 Cu3 N1 . 3_566 91.62(10) y
N18 Cu3 N1 2_546 3_566 91.07(10) y
N16 Cu3 N1 . 3_566 160.58(10) y
N2 N1 Cu1 . . 130.1(2) ?
N2 N1 Cu2 . 3_576 129.3(2) ?
Cu1 N1 Cu2 . 3_576 100.51(13) ?
N3 N2 N1 . . 178.3(4) ?
N5 N4 Cu1 . . 129.5(3) ?
N5 N4 Cu2 . . 126.6(2) ?
Cu1 N4 Cu2 . . 101.45(13) ?
N8 N7 Cu2 . . 125.7(3) ?
N8 N7 Cu3 . . 120.6(2) ?
Cu2 N7 Cu3 . . 99.15(12) ?
N9 N8 N7 . . 177.8(5) ?
N11 N10 Cu2 . . 128.9(2) ?
N11 N10 Cu3 . . 123.3(2) ?
Cu2 N10 Cu3 . . 102.78(13) ?
N12 N11 N10 . . 178.8(4) ?
N14 N13 Cu3 . . 121.0(3) ?
N14 N13 Cu2 . 1_545 122.8(2) ?
Cu3 N13 Cu2 . 1_545 109.72(13) ?
N15 N14 N13 . . 178.6(4) ?
N17 N16 Cu3 . . 155.3(3) ?
N16 N17 N18 . . 177.9(4) ?
N17 N18 Cu3 . 2_556 115.7(3) ?
C1 N19 C2 . . 110.9(3) ?
N19 C1 C2 . 3_557 111.7(3) ?
N19 C2 C1 . 3_557 110.7(3) ?
N4 N5 N6' . . 167.6(11) ?
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 N4 . 1.984(3) y
Cu1 N4 3_576 1.984(3) ?
Cu1 N1 . 1.998(3) y
Cu1 N1 3_576 1.998(3) ?
Cu1 N7 1_565 2.747(3) y
Cu2 N10 . 1.964(3) y
Cu2 N4 . 2.003(3) y
Cu2 N1 3_576 2.016(3) y
Cu2 N7 . 2.021(3) y
Cu2 N13 1_565 2.309(3) y
Cu3 N18 2_546 1.972(3) y
Cu3 N13 . 1.988(3) y
Cu3 N10 . 2.001(3) y
Cu3 N7 . 2.048(3) y
Cu3 N16 . 2.358(3) y
Cu3 N1 3_566 2.942(3) y
N1 N2 . 1.210(4) ?
N1 Cu2 3_576 2.016(3) ?
N2 N3 . 1.139(4) ?
N4 N5 . 1.176(4) ?
N7 N8 . 1.211(4) ?
N8 N9 . 1.141(5) ?
N10 N11 . 1.215(4) ?
N11 N12 . 1.141(4) ?
N13 N14 . 1.201(4) ?
N13 Cu2 1_545 2.309(3) ?
N14 N15 . 1.152(4) ?
N16 N17 . 1.155(4) ?
N17 N18 . 1.201(4) ?
N18 Cu3 2_556 1.972(3) ?
N19 C1 . 1.477(5) ?
N19 C2 . 1.482(4) ?
C1 C2 3_557 1.502(5) ?
C2 C1 3_557 1.502(5) ?
N5 N6' . 1.182(11) ?
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
N19 H1A N18 2_546 0.90 2.23 3.103(4) 163.2
N19 H1B O2 1_445 0.90 1.85 2.738(4) 166.7
O2 H2E N15 4_666 0.85 2.12 2.961(5) 169.5
O2 H2F O1 . 0.85 1.90 2.744(8) 169.2
O2 H2F O1' . 0.85 1.98 2.672(12) 137.5
O1 H1E N6 4_676 0.85 2.20 2.94(2) 145.1
O1 H1F N6 3_666 0.85 2.43 3.19(3) 148.6
O1' H1'A N9 4_666 0.85 2.63 3.034(12) 110.7
O1' H1'B N6' 3_666 0.85 2.05 2.888(14) 170.8
