#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/15/13/7151397.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_7151397
loop_
_publ_author_name
'Kylie N. Brown'
'Rodney J. Geue'
'Trevor W. Hambley'
'David C. R. Hockless'
'A. David Rae'
'Alan M. Sargeson'
_publ_section_title
;
 Specificity in template syntheses of hexaaza-macrobicyclic cages:
 [Pt(Me5-tricosatrieneN6)]4+ and [Pt(Me5-tricosaneN6)]4+
;
_journal_issue                   9
_journal_name_full               'Org. Biomol. Chem.'
_journal_page_first              1598
_journal_page_last               1608
_journal_paper_doi               10.1039/b212326f
_journal_volume                  1
_journal_year                    2003
_chemical_formula_moiety
'(C22 H42 N6 Pt 4+), (Cl4 Zn 2-)1.5, (Cl 1-), 2(H2 O)'
_chemical_formula_sum            'C22 H46 Cl7 N6 O2 Pt Zn1.5'
_chemical_formula_weight         967.98
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_audit_creation_date             1999-06-03
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   14.724(5)
_cell_length_b                   14.724(5)
_cell_length_c                   55.80(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_volume                     10477(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'RAELS96, (Rae, 1996)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device_type  Nonius-CAD4
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6497
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        -8.1
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.573
_exptl_absorpt_correction_T_max  0.408
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Coppens et al (1965)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5736.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.2
_refine_diff_density_min         -0.8
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.932
_refine_ls_goodness_of_fit_ref   1.964
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1480
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/esd_max         0.1
_refine_ls_shift/esd_mean        0.04
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.0016|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1020
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                1480
_reflns_number_total             2066
_reflns_threshold_expression     I>3.00σ(I)
_cod_data_source_file            b212326f.txt
_cod_data_source_block           PTTRIIMINE
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.0016|Fo|^2^]' 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) + 0.0016|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10476(6)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C22 H46 Cl7 N6 O2 Pt1 Zn1.5 '
_cod_database_code               7151397
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -y,-x,1/2+z
5 x,x-y,1/2+z
6 -x+y,y,1/2+z
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 y,x,1/2-z
11 -x,-x+y,1/2-z
12 x-y,-y,1/2-z
13 1/3+x,2/3+y,2/3+z
14 1/3-y,2/3+x-y,2/3+z
15 1/3-x+y,2/3-x,2/3+z
16 1/3-y,2/3-x,7/6+z
17 1/3+x,2/3+x-y,7/6+z
18 1/3-x+y,2/3+y,7/6+z
19 1/3-x,2/3-y,2/3-z
20 1/3+y,2/3-x+y,2/3-z
21 1/3+x-y,2/3+x,2/3-z
22 1/3+y,2/3+x,7/6-z
23 1/3-x,2/3-x+y,7/6-z
24 1/3+x-y,2/3-y,7/6-z
25 2/3+x,1/3+y,1/3+z
26 2/3-y,1/3+x-y,1/3+z
27 2/3-x+y,1/3-x,1/3+z
28 2/3-y,1/3-x,5/6+z
29 2/3+x,1/3+x-y,5/6+z
30 2/3-x+y,1/3+y,5/6+z
31 2/3-x,1/3-y,1/3-z
32 2/3+y,1/3-x+y,1/3-z
33 2/3+x-y,1/3+x,1/3-z
34 2/3+y,1/3+x,5/6-z
35 2/3-x,1/3-x+y,5/6-z
36 2/3+x-y,1/3-y,5/6-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_occupancy
_atom_site_refinement_flags
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Pt1 0.0000 0.0000 0.36249(1) 0.0256(3) 1.0 . Uani d ?
N1 0.1066(6) -0.0081(5) 0.3847(1) 0.033(2) 1.0 . Uani d ?
N2 0.1175(5) 0.1100(5) 0.3407(1) 0.031(2) 1.0 . Uani d ?
C1 0.0000 0.0000 0.4462(4) 0.063(7) 1.0 . Uani d ?
C2 0.0000 0.0000 0.4180(4) 0.040(5) 1.0 . Uani d ?
C3 0.0691(7) -0.0439(7) 0.4097(2) 0.038(2) 1.0 . Uani d ?
C4 0.2015(6) 0.0207(6) 0.3793(2) 0.039(2) 1.0 . Uani d ?
C5 0.2558(7) 0.0720(7) 0.3570(2) 0.041(2) 1.0 . Uani d ?
C6 0.3733(8) 0.1252(9) 0.3586(2) 0.065(3) 1.0 . Uani d ?
C7 0.2256(7) 0.1542(7) 0.3497(2) 0.045(2) 1.0 . Uani d ?
C8 0.1108(8) 0.0746(7) 0.3151(2) 0.036(2) 1.0 . Uani d ?
C9 0.0000 0.0000 0.3066(3) 0.032(4) 1.0 . Uani d ?
C10 0.0000 0.0000 0.2791(4) 0.047(5) 1.0 . Uani d ?
Zn1 0.0326(2) 0.3212(2) 0.2380(1) 0.082(2) 0.5 . Uani d ?
Cl1 0.0045(5) 0.4514(3) 0.2471(1) 0.061(2) 0.5 . Uani d ?
Cl2 0.1088(7) 0.2874(8) 0.2681(1) 0.205(7) 0.5 . Uani d ?
Cl3 0.1399(5) 0.3721(5) 0.2066(1) 0.109(3) 0.5 . Uani d ?
Cl4 -0.1121(4) 0.1815(4) 0.2255(1) 0.165(6) 0.5 . Uani d ?
Cl5 0.1556(6) 0.3219(6) 0.3226(2) 0.063(3) 0.3333 . Uani d ?
O1 0.1472(38) 0.3197(38) 0.3285(13) 0.063(3) 0.1667 . Uani d ?
O2 0.2889(10) 0.2566(8) 0.2585(2) 0.084(6) 0.5 . Uani d ?
H1(O1) 0.1357 0.3111 0.3108 0.063 0.1667 . Uani c ?
H2(O1) 0.2223 0.3719 0.3319 0.063 0.1667 . Uani c ?
H1(O2) 0.2224 0.2588 0.2599 0.084 0.5 . Uani c ?
H2(O2) 0.2797 0.2027 0.2463 0.084 0.5 . Uani c ?
H1(N2) 0.1046 0.1705 0.3400 0.031 1.0 . Uani c ?
H1(C1) -0.0449 0.0285 0.4522 0.063 1.0 . Uani c ?
H1(C3) 0.1309 -0.0184 0.4207 0.038 1.0 . Uani c ?
H2(C3) 0.0278 -0.1222 0.4101 0.038 1.0 . Uani c ?
H1(C4) 0.2430 0.0070 0.3915 0.039 1.0 . Uani c ?
H1(C5) 0.2319 0.0177 0.3441 0.041 1.0 . Uani c ?
H1(C6) 0.4049 0.1583 0.3429 0.065 1.0 . Uani c ?
H2(C6) 0.3988 0.1805 0.3713 0.065 1.0 . Uani c ?
H3(C6) 0.3944 0.0723 0.3628 0.065 1.0 . Uani c ?
H1(C7) 0.2336 0.1982 0.3641 0.045 1.0 . Uani c ?
H2(C7) 0.2749 0.1994 0.3369 0.045 1.0 . Uani c ?
H1(C8) 0.1527 0.0384 0.3135 0.036 1.0 . Uani c ?
H2(C8) 0.1417 0.1380 0.3045 0.036 1.0 . Uani c ?
H1(C10) -0.0725 -0.0488 0.2731 0.047 1.0 . Uani c ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 264 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 552 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 24 0.008 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl 0 84 0.132 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N 0 72 0.004 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Pt 0 12 -2.352 8.388
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Zn 0 18 0.222 1.431
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pt1 N2 92.1(3) . . . yes
N1 Pt1 N1 87.2(3) . . 2_555 yes
N2 Pt1 N2 89.0(3) . . 2_555 yes
N1 Pt1 N2 178.7(2) . . 2_555 yes
N1 Pt1 N2 91.7(3) . . 3_555 yes
Pt1 N1 C3 115.3(6) . . . yes
Pt1 N1 C4 125.5(6) . . . yes
C3 N1 C4 119.0(7) . . . yes
Pt1 N2 C7 116.0(5) . . . yes
Pt1 N2 C8 113.7(5) . . . yes
C7 N2 C8 110.3(6) . . . yes
C1 C2 C3 107.6(8) . . . yes
N1 C3 C2 109.9(10) . . . yes
N1 C4 C5 126.4(8) . . . yes
C4 C5 C6 113.9(8) . . . yes
C4 C5 C7 109.3(6) . . . yes
C6 C5 C7 108.5(8) . . . yes
N2 C7 C5 114.6(7) . . . yes
N2 C8 C9 114.0(9) . . . yes
C8 C9 C10 108.2(8) . . . yes
Cl1 Zn1 Cl2 110.9(3) . . . yes
Cl1 Zn1 Cl3 107.3(3) . . . yes
Cl1 Zn1 Cl4 111.6(3) . . . yes
Cl2 Zn1 Cl3 108.6(3) . . . yes
Cl2 Zn1 Cl4 113.1(3) . . . yes
Cl3 Zn1 Cl4 104.9(3) . . . yes
Zn1 Cl2 Cl5 143.5(4) . . . yes
Zn1 Cl2 O1 141.9(9) . . . yes
Zn1 Cl2 O2 119.5(4) . . . yes
Cl5 Cl2 O2 93.5(3) . . . yes
O1 Cl2 O2 95.8(9) . . . yes
Pt1 N2 Cl5 130.4(3) . . . yes
C3 N2 Cl5 136.4(3) . . . yes
C4 N2 Cl5 139.3(3) . . . yes
Pt1 N2 O1 125.3(12) . . . yes
C3 N2 O1 130.1(14) . . . yes
C4 N2 O1 136.0(12) . . . yes
Pt1 N2 Cl5 119.7(3) . . 19_555 yes
C3 N2 Cl5 114.0(3) . . 19_555 yes
C4 N2 Cl5 118.5(3) . . 19_555 yes
Pt1 N2 O1 125.4(12) . . 19_555 yes
C3 N2 O1 120.1(13) . . 19_555 yes
C4 N2 O1 122.3(11) . . 19_555 yes
N2 Cl5 Cl2 104.1(3) . . . yes
N2 Cl5 Cl2 99.1(3) . 19_555 19_555 yes
N2 O1 Cl2 92.8(16) . 19_555 19_555 yes
Cl2 O2 Cl4 126.3(4) . . 3_555 yes
Cl4 O2 Cl2 126.3(4) . 2_555 2_555 yes
N2 Cl5 Cl4 105.0(3) . . 11_555 yes
N2 O1 Cl4 99.6(17) . . 11_555 yes
N2 Cl5 Cl4 79.8(3) . 19_555 11_555 yes
N2 O1 Cl4 84.8(14) . 19_555 11_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 Pt1 2.050(7) . . yes
N2 Pt1 2.072(6) . . yes
C2 C1 1.575(27) . . yes
C3 N1 1.497(11) . . yes
C3 C2 1.525(12) . . yes
C4 N1 1.277(10) . . yes
C5 C4 1.470(12) . . yes
C6 C5 1.503(13) . . yes
C7 N2 1.475(11) . . yes
C7 C5 1.538(13) . . yes
C8 N2 1.508(11) . . yes
C9 C8 1.517(11) . . yes
C10 C9 1.533(27) . . yes
Cl1 Zn1 2.214(4) . . yes
Cl2 Zn1 2.210(5) . . yes
Cl3 Zn1 2.224(7) . . yes
Cl4 Zn1 2.207(5) . . yes
Cl5 Cl2 3.106(12) . . yes
O1 Cl2 3.414(70) . . yes
O2 Cl2 2.954(14) . . yes
Cl4 O2 2.840(7) . 2_555 yes
O2 Cl4 2.840(7) . 3_555 yes
N2 Cl5 3.052(10) . . yes
N2 O1 2.972(52) . . yes
N2 Cl5 3.115(10) . 19_555 yes
N2 O1 3.113(50) . 19_555 yes
O1 Cl4 3.049(70) . 11_555 yes
Cl4 O1 3.049(70) . 11_555 yes
Cl4 Cl5 3.978(12) . 29_454 yes
Cl4 O1 3.681(69) . 29_454 yes
Cl2 Cl5 4.343(12) . 19_555 yes
Cl4 Cl5 2.742(12) . 11_555 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 Pt1 N2 155.7(5) . . . . no
C4 N1 Pt1 N2 -19.6(7) . . . . no
C7 N2 Pt1 N1 -9.4(6) . . . . no
C8 N2 Pt1 N1 120.0(5) . . . . no
C2 C3 N1 Pt1 -37.0(8) . . . . no
C2 C3 N1 C4 138.6(8) . . . . no
C5 C4 N1 Pt1 4.6(12) . . . . no
C5 C4 N1 C3 -170.5(8) . . . . no
C5 C7 N2 Pt1 52.7(8) . . . . no
C5 C7 N2 C8 -78.3(8) . . . . no
C9 C8 N2 Pt1 30.4(8) . . . . no
C9 C8 N2 C7 162.7(7) . . . . no
N1 C3 C2 C1 202.2(5) . . . . no
C6 C5 C4 N1 162.5(9) . . . . no
C7 C5 C4 N1 41.1(12) . . . . no
N2 C7 C5 C4 -72.1(9) . . . . no
N2 C7 C5 C6 163.2(8) . . . . no
C10 C9 C8 N2 -198.9(5) . . . . no
O1 Cl2 Zn1 Cl1 21.1(15) . . . . no
O1 Cl2 Zn1 Cl3 138.8(14) . . . . no
O1 Cl2 Zn1 Cl4 -105.1(14) . . . . no
