#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:20:21 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179625 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/89/4508913.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4508913
loop_
_publ_author_name
'Luisi, Brian S.'
'Kravtsov, Victor Ch.'
'Moulton, Brian D.'
_publ_section_title
;
 An (8,3)-a 3D Coordination Network and Concomitant Three-Connected
 Supramolecular Isomers
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2207
_journal_paper_doi               10.1021/cg060534x
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C17.27 H20 Cu N3 O7.27'
_chemical_formula_weight         449.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           133
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2b'
_symmetry_space_group_name_H-M   'P 42/n b c :2'
_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                   21.435(2)
_cell_length_b                   21.435(2)
_cell_length_c                   11.382(2)
_cell_measurement_temperature    90(2)
_cell_volume                     5229.6(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43143
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1854
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.135
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.475
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2311
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.493
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3207
_refine_ls_wR_factor_ref         0.3515
_reflns_number_gt                1632
_reflns_number_total             2311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060534xsup2.cif
_cod_data_source_block           bl21sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5229.8(13)
_cod_original_sg_symbol_H-M      P4(2)/nbc
_cod_database_code               4508913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z+1/2'
'y, -x+1/2, z+1/2'
'-x+1/2, y, -z'
'x, -y+1/2, -z'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z-1/2'
'-y, x-1/2, -z-1/2'
'x-1/2, -y, z'
'-x, y-1/2, z'
'-y, -x, z-1/2'
'y-1/2, x-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.2500 0.93806(4) 1.0000 0.0420(6) Uani 1 2 d S
O1 O 0.2987(2) 0.87622(17) 0.9207(4) 0.0522(13) Uani 1 1 d .
N1 N 0.2024(2) 1.0032(2) 1.0900(5) 0.0414(12) Uani 1 1 d .
C1 C 0.1760(3) 1.0529(3) 1.0379(6) 0.0437(15) Uani 1 1 d .
H1 H 0.1828 1.0589 0.9581 0.052 Uiso 1 1 calc R
C2 C 0.1395(3) 1.0952(3) 1.0969(5) 0.0415(14) Uani 1 1 d .
H2 H 0.1227 1.1294 1.0579 0.050 Uiso 1 1 calc R
C3 C 0.1278(2) 1.0859(2) 1.2162(5) 0.0358(13) Uani 1 1 d .
C4 C 0.1556(3) 1.0346(3) 1.2712(6) 0.0411(15) Uani 1 1 d .
H4 H 0.1497 1.0273 1.3509 0.049 Uiso 1 1 calc R
C5 C 0.1920(3) 0.9952(2) 1.2043(6) 0.0413(15) Uani 1 1 d .
H5 H 0.2102 0.9611 1.2411 0.050 Uiso 1 1 calc R
C6 C 0.2934(3) 0.8162(2) 0.9314(5) 0.0409(14) Uani 1 1 d .
C7 C 0.2500 0.7854(3) 1.0000 0.0337(18) Uani 1 2 d S
C8 C 0.3413(3) 0.7813(3) 0.8582(5) 0.0454(15) Uani 1 1 d .
H8A H 0.3506 0.8048 0.7887 0.068 Uiso 1 1 calc R
H8B H 0.3249 0.7412 0.8364 0.068 Uiso 1 1 calc R
H8C H 0.3788 0.7756 0.9033 0.068 Uiso 1 1 calc R
O1M O 0.1685(3) 0.9452(3) 0.8455(5) 0.0828(19) Uani 1 1 d .
C1M C 0.1092(7) 0.9218(8) 0.8577(19) 0.174(7) Uani 1 1 d .
H1M1 H 0.0880 0.9437 0.9195 0.261 Uiso 1 1 calc R
H1M2 H 0.1114 0.8782 0.8769 0.261 Uiso 1 1 calc R
H1M3 H 0.0868 0.9270 0.7854 0.261 Uiso 1 1 calc R
O2M O 0.1413(7) 0.1413(7) 0.7500 0.050 Uiso 0.272(12) 2 d SP
C2M C 0.1900(11) 0.1900(11) 0.7500 0.050 Uiso 0.272(12) 2 d SP
N1K N 0.0391(6) 0.2157(8) 0.9430(16) 0.131(8) Uani 0.50 1 d PD
O1K O -0.0083(5) 0.2500 1.0000 0.153(6) Uani 1 2 d SD
O2K O 0.0282(7) 0.1719(6) 0.8557(14) 0.114(5) Uani 0.50 1 d PD
O3K O 0.0987(7) 0.2381(15) 0.964(2) 0.168(16) Uani 0.50 1 d PD
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
O1 Cu1 O1 92.3(2) . 5_557
O1 Cu1 N1 87.96(18) . 5_557
O1 Cu1 N1 176.9(2) 5_557 5_557
O1 Cu1 N1 176.9(2) . .
O1 Cu1 N1 87.96(18) 5_557 .
N1 Cu1 N1 91.9(3) 5_557 .
C6 O1 Cu1 126.5(3) . .
C5 N1 C1 117.5(5) . .
C5 N1 Cu1 119.6(4) . .
C1 N1 Cu1 122.7(4) . .
N1 C1 C2 123.2(6) . .
C1 C2 C3 118.9(5) . .
C2 C3 C4 118.2(5) . .
C2 C3 C3 121.7(6) . 7_467
C4 C3 C3 120.1(6) . 7_467
C5 C4 C3 118.4(6) . .
N1 C5 C4 123.8(6) . .
O1 C6 C7 125.8(5) . .
O1 C6 C8 112.2(5) . .
C7 C6 C8 122.0(5) . .
C6 C7 C6 123.0(7) . 5_557
C6 C7 C7 118.5(3) . 2_565
C6 C7 C7 118.5(3) 5_557 2_565
O3K N1K O2K 120.7(12) . .
O3K N1K O1K 114.0(11) . .
O2K N1K O1K 124.1(10) . .
N1K O1K N1K 87.9(13) . 6_557
O3K O3K N1K 109.0(13) 6_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.914(4) .
Cu1 O1 1.914(4) 5_557
Cu1 N1 2.010(4) 5_557
Cu1 N1 2.010(4) .
O1 C6 1.298(6) .
N1 C5 1.331(8) .
N1 C1 1.343(7) .
C1 C2 1.373(8) .
C2 C3 1.395(9) .
C3 C4 1.398(8) .
C3 C3 1.487(10) 7_467
C4 C5 1.378(8) .
C6 C7 1.383(7) .
C6 C8 1.519(8) .
C7 C6 1.383(7) 5_557
C7 C7 1.518(14) 2_565
O1M C1M 1.374(16) .
O2M C2M 1.48(4) .
N1K O3K 1.384(15) .
N1K O2K 1.387(14) .
N1K O1K 1.412(13) .
O1K N1K 1.412(13) 6_557
O3K O3K 0.98(4) 6_557
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Cu1 O1 C6 -1.0(4) 5_557 .
N1 Cu1 O1 C6 -177.9(5) 5_557 .
N1 Cu1 O1 C6 94(3) . .
O1 Cu1 N1 C5 -51(3) . .
O1 Cu1 N1 C5 44.1(4) 5_557 .
N1 Cu1 N1 C5 -139.0(5) 5_557 .
O1 Cu1 N1 C1 134(3) . .
O1 Cu1 N1 C1 -130.5(5) 5_557 .
N1 Cu1 N1 C1 46.4(4) 5_557 .
C5 N1 C1 C2 0.2(9) . .
Cu1 N1 C1 C2 174.9(4) . .
N1 C1 C2 C3 -1.3(9) . .
C1 C2 C3 C4 1.9(8) . .
C1 C2 C3 C3 -176.6(4) . 7_467
C2 C3 C4 C5 -1.3(8) . .
C3 C3 C4 C5 177.1(4) 7_467 .
C1 N1 C5 C4 0.3(8) . .
Cu1 N1 C5 C4 -174.5(4) . .
C3 C4 C5 N1 0.3(8) . .
Cu1 O1 C6 C7 2.0(9) . .
Cu1 O1 C6 C8 -178.1(4) . .
O1 C6 C7 C6 -1.1(5) . 5_557
C8 C6 C7 C6 179.0(6) . 5_557
O1 C6 C7 C7 178.9(5) . 2_565
C8 C6 C7 C7 -1.0(6) . 2_565
O3K N1K O1K N1K -6.4(15) . 6_557
O2K N1K O1K N1K -174(2) . 6_557
O2K N1K O3K O3K -169(4) . 6_557
O1K N1K O3K O3K 23(5) . 6_557
