#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:53:28 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232960 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/84/4348460.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_4348460
loop_
_publ_author_name
'Ahmed, Basil M.'
'Mezei, Gellert'
_publ_section_title
;
 From Ordinary to Extraordinary: Insights into the Formation Mechanism and
 pH-Dependent Assembly/Disassembly of Nanojars.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7717
_journal_page_last               7728
_journal_paper_doi               10.1021/acs.inorgchem.6b01172
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C11 H13 Cu3 N9 O7'
_chemical_formula_weight         573.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.44660(10)
_cell_length_b                   11.44660(10)
_cell_length_c                   14.7076(2)
_cell_measurement_reflns_used    9459
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.25
_cell_volume                     1927.06(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.957
_diffrn_reflns_theta_min         2.255
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 827 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3323
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0261P)²+0.5730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2322
_reflns_number_total             3323
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01172_si_002.cif
_cod_data_source_block           1b
_cod_database_code               4348460
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.19148(3) 0.19148(3) 0.0000 0.05483(16) Uani 1 2 d S T P . .
Cu2 Cu 0.46779(4) 0.27381(4) 0.03733(3) 0.05660(13) Uani 1 1 d D . . . .
O1 O 0.3181(4) 0.3050(4) -0.0342(3) 0.0488(9) Uani 0.5 1 d D . P A -1
H1O H 0.327(7) 0.280(6) -0.086(3) 0.059 Uiso 0.5 1 d D U P B -1
N1 N 0.3083(3) 0.0807(2) 0.0438(2) 0.0557(6) Uani 1 1 d . . . . .
N2 N 0.4175(3) 0.1177(3) 0.0641(2) 0.0561(7) Uani 1 1 d . . . . .
N3 N 0.5135(3) 0.4319(3) 0.0099(2) 0.0624(8) Uani 1 1 d . . . . .
N4A N 0.6807(9) 0.1883(9) 0.0056(8) 0.055(2) Uani 0.5 1 d D . P A 1
O2A O 0.6256(11) 0.2359(15) 0.0708(7) 0.061(2) Uani 0.5 1 d D . P A 1
O3A O 0.7686(6) 0.1340(6) 0.0295(5) 0.0729(16) Uani 0.5 1 d D . P A 1
O4A O 0.6429(8) 0.1926(9) -0.0712(5) 0.083(2) Uani 0.5 1 d D . P A 1
N4B N 0.7037(8) 0.1826(9) 0.0501(6) 0.063(2) Uani 0.5 1 d D . P A 2
O2B O 0.6301(11) 0.2434(16) 0.1022(7) 0.062(3) Uani 0.5 1 d D . P A 2
O3B O 0.7920(6) 0.1433(7) 0.0859(6) 0.085(2) Uani 0.5 1 d D . P A 2
O4B O 0.6807(13) 0.1752(13) -0.0313(7) 0.095(4) Uani 0.5 1 d D . P A 2
N5 N 0.0663(3) 0.0663(3) 0.0000 0.0640(11) Uani 1 2 d S T P A .
C1 C 0.4767(4) 0.0249(4) 0.0966(3) 0.0679(9) Uani 1 1 d . . . . .
H1 H 0.5539 0.0265 0.1164 0.082 Uiso 1 1 calc R U . . .
C2 C 0.4074(4) -0.0710(4) 0.0961(3) 0.0686(10) Uani 1 1 d . . . . .
H2 H 0.4269 -0.1462 0.1146 0.082 Uiso 1 1 calc R U . . .
C3 C 0.3023(3) -0.0334(3) 0.0625(3) 0.0649(9) Uani 1 1 d . . . . .
H3 H 0.2367 -0.0801 0.0540 0.078 Uiso 1 1 calc R U . . .
C4 C 0.6165(4) 0.4856(4) 0.0166(3) 0.0816(14) Uani 1 1 d . . . . .
H4 H 0.6870 0.4494 0.0304 0.098 Uiso 1 1 calc R U . . .
C5 C 0.6022(4) 0.6022(4) 0.0000 0.099(2) Uani 1 2 d S T P . .
H5 H 0.6596 0.6596 0.0000 0.119 Uiso 1 2 calc R U P . .
C6 C -0.0029(3) -0.0029(3) 0.0000 0.0601(12) Uani 1 2 d S T P . .
C7 C -0.0921(4) -0.0921(4) 0.0000 0.089(2) Uani 1 2 d S T P A .
H7A H -0.1661 -0.0577 0.0150 0.134 Uiso 0.5 1 calc R U P . .
H7B H -0.0730 -0.1508 0.0442 0.134 Uiso 0.5 1 calc R U P . .
H7C H -0.0966 -0.1272 -0.0592 0.134 Uiso 0.5 1 calc R U P . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Cu1 N1 177.17(17) . 7
N1 Cu1 O1 90.50(17) . .
N1 Cu1 O1 86.76(15) 7 .
N1 Cu1 N5 91.42(8) . .
N1 Cu1 N5 91.42(8) 7 .
O1 Cu1 N5 165.18(12) . .
N1 Cu1 O2B 95.9(4) . 4_455
N1 Cu1 O2B 84.0(4) 7 4_455
N5 Cu1 O2B 90.7(3) . 4_455
N1 Cu1 O2B 84.0(4) . 2_544
N1 Cu1 O2B 95.9(4) 7 2_544
N5 Cu1 O2B 90.7(3) . 2_544
O2B Cu1 O2B 178.6(7) 4_455 2_544
N2 Cu2 O2A 91.1(6) . .
N2 Cu2 N3 178.29(13) . .
O2A Cu2 N3 90.6(6) . .
N2 Cu2 O1 90.97(15) . .
O2A Cu2 O1 163.7(3) . .
N3 Cu2 O1 87.47(15) . .
N2 Cu2 O2B 91.0(5) . .
N3 Cu2 O2B 90.6(5) . .
Cu1 O1 Cu2 111.3(2) . .
Cu1 O1 H1O 96(5) . .
Cu2 O1 H1O 108(5) . .
C3 N1 N2 107.9(3) . .
C3 N1 Cu1 131.9(3) . .
N2 N1 Cu1 120.1(2) . .
C1 N2 N1 107.3(3) . .
C1 N2 Cu2 131.0(3) . .
N1 N2 Cu2 121.6(2) . .
C4 N3 N3 107.9(3) . 7
C4 N3 Cu2 131.1(3) . .
N3 N3 Cu2 120.41(10) 7 .
O4A N4A O3A 125.3(10) . .
O4A N4A O2A 120.7(10) . .
O3A N4A O2A 113.9(12) . .
N4A O2A Cu2 111.7(7) . .
O3B N4B O4B 124.8(12) . .
O3B N4B O2B 117.7(9) . .
O4B N4B O2B 117.4(11) . .
N4B O2B Cu2 112.4(6) . .
N4B O2B Cu1 119.8(8) . 3
Cu2 O2B Cu1 127.8(5) . 3
C6 N5 Cu1 180.0(4) . .
C2 C1 N2 110.0(4) . .
C2 C1 H1 125.0 . .
N2 C1 H1 125.0 . .
C1 C2 C3 105.2(4) . .
C1 C2 H2 127.4 . .
C3 C2 H2 127.4 . .
N1 C3 C2 109.7(4) . .
N1 C3 H3 125.2 . .
C2 C3 H3 125.2 . .
N3 C4 C5 109.4(5) . .
N3 C4 H4 125.3 . .
C5 C4 H4 125.3 . .
C4 C5 C4 105.4(6) . 7
C4 C5 H5 127.3 . .
C4 C5 H5 127.3 7 .
N5 C6 C7 180.0(6) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.952(3) .
Cu1 N1 1.952(3) 7
Cu1 O1 2.011(4) .
Cu1 N5 2.027(4) .
Cu1 O2B 2.403(8) 4_455
Cu1 O2B 2.403(8) 2_544
Cu2 N2 1.919(3) .
Cu2 O2A 1.922(12) .
Cu2 N3 1.927(3) .
Cu2 O1 2.042(5) .
Cu2 O2B 2.117(12) .
O1 H1O 0.82(3) .
N1 C3 1.336(4) .
N1 N2 1.354(4) .
N2 C1 1.347(5) .
N3 C4 1.333(5) .
N3 N3 1.352(7) 7
N4A O4A 1.211(12) .
N4A O3A 1.234(12) .
N4A O2A 1.270(13) .
N4B O3B 1.225(11) .
N4B O4B 1.228(11) .
N4B O2B 1.335(14) .
O2B Cu1 2.403(8) 3
N5 C6 1.120(7) .
C1 C2 1.355(6) .
C1 H1 0.9300 .
C2 C3 1.370(6) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C5 1.366(6) .
C4 H4 0.9300 .
C5 C4 1.366(6) 7
C5 H5 0.9300 .
C6 C7 1.444(8) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
