#------------------------------------------------------------------------------
#$Date: 2017-03-02 17:12:34 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/44/7024408.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_7024408
loop_
_publ_author_name
'Schilter, David'
'Clegg, Jack K.'
'Harding, Margaret M.'
'Rendina, Louis M.'
_publ_section_title
;
 Platinum(II) and palladium(II) metallomacrocycles derived from cationic
 4,4'-bipyridinium, 3-aminopyrazinium and 2-aminopyrimidinium ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              239
_journal_page_last               247
_journal_paper_doi               10.1039/b916579g
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C5 H8 N3, N O3'
_chemical_formula_sum            'C5 H8 N4 O3'
_chemical_formula_weight         172.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   6.1596(7)
_cell_length_b                   6.1596(7)
_cell_length_c                   16.966(4)
_cell_measurement_reflns_used    4414
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.281
_cell_measurement_theta_min      3.603
_cell_volume                     557.46(16)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 1995)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)'
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5431
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        16
_diffrn_standards_number         88
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.570
_exptl_crystal_size_min          0.560
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881 863 Friedel pairs'
_refine_ls_abs_structure_Flack   0.074(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1771
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0266
_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)+(0.0509P)²+0.0552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                1740
_reflns_number_total             1771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b916579g.txt
_cod_data_source_block           lj128sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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:
data name '_intl_tables_symmetry_no' replaced with
'_symmetry_Int_Tables_number' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_sg_symbol_H-M      P32
_cod_database_code               7024408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
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
C1 C 0.87653(19) 1.0515(2) 0.45601(6) 0.0198(2) Uani 1 1 d .
C2 C 0.84052(19) 0.9819(2) 0.53659(6) 0.0200(2) Uani 1 1 d .
H2 H 0.9079 1.1063 0.5766 0.024 Uiso 1 1 calc R
C3 C 0.6176(2) 0.5598(2) 0.49946(7) 0.0232(2) Uani 1 1 d .
H3 H 0.5264 0.3871 0.5130 0.028 Uiso 1 1 calc R
C4 C 0.6599(2) 0.6369(2) 0.42181(7) 0.0249(2) Uani 1 1 d .
H4 H 0.5953 0.5115 0.3821 0.030 Uiso 1 1 calc R
C5 C 0.6645(2) 0.6667(2) 0.63976(7) 0.0264(2) Uani 1 1 d .
H5A H 0.8245 0.7415 0.6681 0.040 Uiso 1 1 calc R
H5B H 0.5804 0.4837 0.6441 0.040 Uiso 1 1 calc R
H5C H 0.5578 0.7263 0.6628 0.040 Uiso 1 1 calc R
N1 N 0.78529(18) 0.87523(18) 0.39895(5) 0.0224(2) Uani 1 1 d .
N2 N 0.71126(16) 0.74043(17) 0.55540(5) 0.01972(19) Uani 1 1 d .
N3 N 1.0033(2) 1.29276(19) 0.43481(7) 0.0272(2) Uani 1 1 d .
N4 N 0.27151(17) 0.84219(18) 0.55295(5) 0.0212(2) Uani 1 1 d .
O1 O 0.28518(18) 0.87747(19) 0.48034(5) 0.0317(2) Uani 1 1 d .
O2 O 0.38799(19) 1.02401(16) 0.59906(5) 0.0330(2) Uani 1 1 d .
O3 O 0.14361(16) 0.62536(17) 0.58022(5) 0.02875(19) Uani 1 1 d .
H1N H 1.024(3) 1.329(3) 0.3878(14) 0.035 Uiso 1 1 d .
H2N H 1.050(3) 1.410(4) 0.4699(11) 0.035 Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0173(4) 0.0223(5) 0.0210(5) -0.0010(4) -0.0004(3) 0.0107(4)
C2 0.0189(5) 0.0221(5) 0.0194(5) -0.0030(4) -0.0017(4) 0.0106(4)
C3 0.0227(5) 0.0200(5) 0.0255(6) -0.0006(4) -0.0016(4) 0.0095(4)
C4 0.0255(5) 0.0230(5) 0.0249(6) -0.0050(4) -0.0038(4) 0.0112(4)
C5 0.0282(6) 0.0355(6) 0.0173(6) 0.0055(4) 0.0014(4) 0.0173(5)
N1 0.0236(4) 0.0233(4) 0.0192(4) -0.0015(3) -0.0013(3) 0.0108(4)
N2 0.0173(4) 0.0246(4) 0.0187(4) 0.0014(3) -0.0004(3) 0.0116(4)
N3 0.0317(5) 0.0206(5) 0.0234(5) 0.0000(4) 0.0002(4) 0.0085(4)
N4 0.0222(4) 0.0268(4) 0.0204(4) 0.0002(3) 0.0010(3) 0.0165(4)
O1 0.0365(5) 0.0448(5) 0.0184(4) 0.0035(4) 0.0007(3) 0.0236(4)
O2 0.0448(5) 0.0259(4) 0.0270(4) -0.0058(3) 0.0012(4) 0.0168(4)
O3 0.0279(4) 0.0255(4) 0.0309(4) 0.0036(3) 0.0019(3) 0.0118(3)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N3 C1 N1 118.56(10)
N3 C1 C2 120.79(10)
N1 C1 C2 120.65(10)
N2 C2 C1 119.08(9)
N2 C2 H2 120.5
C1 C2 H2 120.5
N2 C3 C4 117.20(10)
N2 C3 H3 121.4
C4 C3 H3 121.4
N1 C4 C3 124.32(10)
N1 C4 H4 117.8
C3 C4 H4 117.8
N2 C5 H5A 109.5
N2 C5 H5B 109.5
H5A C5 H5B 109.5
N2 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
C4 N1 C1 117.20(10)
C2 N2 C3 121.53(10)
C2 N2 C5 119.33(9)
C3 N2 C5 119.13(9)
C1 N3 H1N 119.2(13)
C1 N3 H2N 120.5(12)
H1N N3 H2N 120.0(17)
O1 N4 O3 120.21(10)
O1 N4 O2 120.10(10)
O3 N4 O2 119.69(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N3 1.3370(15)
C1 N1 1.3496(13)
C1 C2 1.4167(15)
C2 N2 1.3281(14)
C2 H2 0.9500
C3 N2 1.3525(15)
C3 C4 1.3804(17)
C3 H3 0.9500
C4 N1 1.3295(14)
C4 H4 0.9500
C5 N2 1.4857(15)
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
N3 H1N 0.82(2)
N3 H2N 0.867(19)
N4 O1 1.2464(12)
N4 O3 1.2515(14)
N4 O2 1.2560(13)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H1N O2 0.82(2) 2.12(2) 2.9195(16) 165.4(18) 2_774
N3 H2N O3 0.867(19) 2.198(19) 3.0431(15) 165.0(17) 1_665
N3 H2N O1 0.867(19) 2.500(19) 3.2139(15) 140.1(15) 1_665
N3 H2N N4 0.867(19) 2.702(19) 3.5509(15) 166.5(16) 1_665
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
N3 C1 C2 N2 179.29(9)
N1 C1 C2 N2 -1.30(14)
N2 C3 C4 N1 -0.16(17)
C3 C4 N1 C1 0.12(16)
N3 C1 N1 C4 -179.97(10)
C2 C1 N1 C4 0.60(15)
C1 C2 N2 C3 1.27(14)
C1 C2 N2 C5 -177.67(9)
C4 C3 N2 C2 -0.57(15)
C4 C3 N2 C5 178.37(10)
