#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/37/7103726.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_7103726
loop_
_publ_author_name
'Martin Schroder'
'Alexander J. Blake'
'Neil Champness'
'Caitlin J. Horn'
'Vito Lippolis'
_publ_section_title
;
Construction of the first cross-linked double
helical polyiodide
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b303289b
_journal_year                    2003
_chemical_formula_moiety         'C44 H36 N16 Zn2, 4(I3), 3(I2)'
_chemical_formula_sum            'C44 H36 I18 N16 Zn2'
_chemical_formula_weight         3203.87
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 107.268(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.505(2)
_cell_length_b                   11.280(1)
_cell_length_c                   21.938(2)
_cell_measurement_reflns_used    9278
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.27
_cell_volume                     3664(1)
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.035
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22781
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.281
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS version 2.03; Bruker, 2001)'
_exptl_crystal_colour            Red-black
_exptl_crystal_density_diffrn    2.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.21
_refine_diff_density_min         -2.35
_refine_diff_density_rms         0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0348P)²+16.20P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                6774
_reflns_number_total             8505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303289b.txt
_cod_data_source_block           ZNI8PY
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometrically placed' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7103726
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.65664(3) 1.26162(4) 0.70876(2) 0.03488(11) Uani 1 1 d . . .
I2 I 0.63446(3) 1.20194(4) 0.82443(3) 0.03959(12) Uani 1 1 d . . .
I3 I 0.59340(4) 1.19579(4) 0.97376(2) 0.03865(12) Uani 1 1 d . . .
I4 I 0.75216(3) 1.02928(5) 1.01037(2) 0.04048(13) Uani 1 1 d . . .
I5 I 0.89967(4) 0.86649(7) 1.04055(3) 0.0673(2) Uani 1 1 d . . .
I6 I 1.05845(3) 0.70800(4) 0.97499(2) 0.03848(12) Uani 1 1 d . . .
I7 I 1.18284(3) 0.54003(4) 0.94997(2) 0.03617(12) Uani 1 1 d . . .
I8 I 1.31609(3) 0.35674(4) 0.93208(2) 0.03735(12) Uani 1 1 d . . .
I9 I 1.01370(3) 0.75098(4) 0.814422(19) 0.02530(9) Uani 1 1 d . . .
Zn1 Zn 0.68138(4) 0.72811(5) 0.77365(3) 0.01413(13) Uani 1 1 d . . .
N1 N 0.5735(3) 0.6258(4) 0.7058(2) 0.0144(9) Uani 1 1 d . . .
N2 N 0.6490(3) 0.6893(4) 0.6340(2) 0.0177(10) Uani 1 1 d . . .
H2A H 0.6627 0.6819 0.5980 0.021 Uiso 1 1 calc R . .
N3 N 0.6956(3) 0.7613(4) 0.6818(2) 0.0150(9) Uani 1 1 d . . .
N4 N 0.7734(3) 0.8817(4) 0.7851(2) 0.0183(10) Uani 1 1 d . . .
N5 N 0.5893(3) 0.8245(4) 0.8161(2) 0.0154(9) Uani 1 1 d . . .
N6 N 0.6888(3) 0.7564(4) 0.9107(2) 0.0199(10) Uani 1 1 d . . .
H6A H 0.7121 0.7585 0.9525 0.024 Uiso 1 1 calc R . .
N7 N 0.7280(3) 0.6931(4) 0.8731(2) 0.0169(9) Uani 1 1 d . . .
N8 N 0.7865(3) 0.5863(4) 0.7871(2) 0.0152(9) Uani 1 1 d . . .
C1 C 0.5018(4) 0.5702(4) 0.7164(3) 0.0142(10) Uani 1 1 d . . .
C2 C 0.4348(4) 0.5158(5) 0.6685(3) 0.0196(12) Uani 1 1 d . . .
H2B H 0.3851 0.4786 0.6777 0.024 Uiso 1 1 calc R . .
C3 C 0.4415(4) 0.5163(5) 0.6069(3) 0.0229(12) Uani 1 1 d . . .
H3A H 0.3970 0.4777 0.5735 0.028 Uiso 1 1 calc R . .
C4 C 0.5133(4) 0.5734(5) 0.5943(3) 0.0220(12) Uani 1 1 d . . .
H4A H 0.5189 0.5758 0.5524 0.026 Uiso 1 1 calc R . .
C5 C 0.5776(3) 0.6277(5) 0.6458(2) 0.0151(10) Uani 1 1 d . . .
C6 C 0.7531(4) 0.8391(5) 0.6752(3) 0.0188(11) Uani 1 1 d . . .
H6B H 0.7674 0.8488 0.6363 0.023 Uiso 1 1 calc R . .
C7 C 0.7947(4) 0.9112(5) 0.7314(3) 0.0194(11) Uani 1 1 d . . .
C8 C 0.8509(4) 1.0050(5) 0.7288(3) 0.0273(13) Uani 1 1 d . . .
H8A H 0.8639 1.0242 0.6903 0.033 Uiso 1 1 calc R . .
C9 C 0.8883(5) 1.0710(6) 0.7847(4) 0.0385(17) Uani 1 1 d . . .
H9A H 0.9278 1.1354 0.7847 0.046 Uiso 1 1 calc R . .
C10 C 0.8669(4) 1.0414(6) 0.8398(4) 0.0339(16) Uani 1 1 d . . .
H10A H 0.8910 1.0851 0.8781 0.041 Uiso 1 1 calc R . .
C11 C 0.8091(4) 0.9460(6) 0.8374(3) 0.0259(13) Uani 1 1 d . . .
H11A H 0.7944 0.9257 0.8752 0.031 Uiso 1 1 calc R . .
C12 C 0.5125(3) 0.8832(4) 0.7857(2) 0.0143(10) Uani 1 1 d . . .
C13 C 0.4579(4) 0.9383(5) 0.8166(3) 0.0198(12) Uani 1 1 d . . .
H13A H 0.4050 0.9797 0.7935 0.024 Uiso 1 1 calc R . .
C14 C 0.4832(4) 0.9310(5) 0.8834(3) 0.0215(12) Uani 1 1 d . . .
H14A H 0.4482 0.9695 0.9064 0.026 Uiso 1 1 calc R . .
C15 C 0.5584(4) 0.8683(5) 0.9151(3) 0.0198(12) Uani 1 1 d . . .
H15A H 0.5750 0.8596 0.9602 0.024 Uiso 1 1 calc R . .
C16 C 0.6107(4) 0.8170(5) 0.8800(3) 0.0175(11) Uani 1 1 d . . .
C17 C 0.7973(4) 0.6269(5) 0.8959(3) 0.0212(12) Uani 1 1 d . . .
H17A H 0.8262 0.6207 0.9405 0.025 Uiso 1 1 calc R . .
C18 C 0.8290(4) 0.5615(5) 0.8491(3) 0.0210(12) Uani 1 1 d . . .
C19 C 0.8983(4) 0.4788(5) 0.8672(3) 0.0271(13) Uani 1 1 d . . .
H19A H 0.9274 0.4629 0.9110 0.033 Uiso 1 1 calc R . .
C20 C 0.9241(4) 0.4198(6) 0.8197(3) 0.0307(14) Uani 1 1 d . . .
H20A H 0.9717 0.3633 0.8307 0.037 Uiso 1 1 calc R . .
C21 C 0.8803(4) 0.4440(6) 0.7566(3) 0.0291(14) Uani 1 1 d . . .
H21A H 0.8963 0.4038 0.7234 0.035 Uiso 1 1 calc R . .
C22 C 0.8123(4) 0.5284(5) 0.7426(3) 0.0225(12) Uani 1 1 d . . .
H22A H 0.7826 0.5458 0.6990 0.027 Uiso 1 1 calc R . .
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
I5 I4 I3 177.76(2) . . ?
I6 I7 I8 176.36(2) . . ?
N7 Zn1 N3 155.29(17) . . ?
N7 Zn1 N1 123.74(17) . . ?
N3 Zn1 N1 73.92(17) . . ?
N7 Zn1 N5 73.97(17) . . ?
N3 Zn1 N5 125.12(17) . . ?
N1 Zn1 N5 94.98(16) . . ?
N7 Zn1 N4 91.01(17) . . ?
N3 Zn1 N4 74.01(17) . . ?
N1 Zn1 N4 145.17(17) . . ?
N5 Zn1 N4 92.43(17) . . ?
N7 Zn1 N8 73.68(17) . . ?
N3 Zn1 N8 88.53(16) . . ?
N1 Zn1 N8 95.24(16) . . ?
N5 Zn1 N8 146.34(16) . . ?
N4 Zn1 N8 97.19(17) . . ?
C5 N1 C1 117.2(4) . . ?
C5 N1 Zn1 114.1(3) . . ?
C1 N1 Zn1 128.5(3) . . ?
N3 N2 C5 115.2(4) . . ?
C6 N3 N2 123.3(5) . . ?
C6 N3 Zn1 119.8(4) . . ?
N2 N3 Zn1 116.6(3) . . ?
C11 N4 C7 117.9(5) . . ?
C11 N4 Zn1 127.9(4) . . ?
C7 N4 Zn1 114.2(4) . . ?
C16 N5 C12 116.9(4) . . ?
C16 N5 Zn1 114.8(4) . . ?
C12 N5 Zn1 128.2(3) . . ?
N7 N6 C16 116.7(4) . . ?
C17 N7 N6 122.8(5) . . ?
C17 N7 Zn1 120.0(4) . . ?
N6 N7 Zn1 116.6(3) . . ?
C22 N8 C18 118.2(5) . . ?
C22 N8 Zn1 128.3(4) . . ?
C18 N8 Zn1 113.5(3) . . ?
N1 C1 C2 123.0(5) . . ?
N1 C1 C1 116.3(5) . 2_656 ?
C2 C1 C1 120.7(5) . 2_656 ?
C1 C2 C3 118.9(5) . . ?
C4 C3 C2 119.6(5) . . ?
C3 C4 C5 117.6(5) . . ?
N1 C5 N2 117.6(5) . . ?
N1 C5 C4 123.7(5) . . ?
N2 C5 C4 118.7(5) . . ?
N3 C6 C7 115.6(5) . . ?
N4 C7 C8 122.9(6) . . ?
N4 C7 C6 115.9(5) . . ?
C8 C7 C6 121.2(5) . . ?
C7 C8 C9 118.2(6) . . ?
C10 C9 C8 119.3(6) . . ?
C9 C10 C11 118.2(6) . . ?
N4 C11 C10 123.5(6) . . ?
N5 C12 C13 123.8(5) . . ?
N5 C12 C12 115.6(5) . 2_656 ?
C13 C12 C12 120.6(5) . 2_656 ?
C12 C13 C14 117.7(5) . . ?
C15 C14 C13 119.7(5) . . ?
C14 C15 C16 118.7(5) . . ?
N5 C16 N6 116.7(5) . . ?
N5 C16 C15 123.1(5) . . ?
N6 C16 C15 120.2(5) . . ?
N7 C17 C18 115.9(5) . . ?
N8 C18 C19 122.1(5) . . ?
N8 C18 C17 115.8(5) . . ?
C19 C18 C17 122.1(5) . . ?
C18 C19 C20 118.5(6) . . ?
C21 C20 C19 119.6(6) . . ?
C20 C21 C22 118.3(6) . . ?
N8 C22 C21 123.3(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.7439(7) . ?
I3 I4 3.0097(8) . ?
I4 I5 2.8535(9) . ?
I6 I7 2.8705(8) . ?
I7 I8 3.0296(7) . ?
I9 I9 2.7308(8) 2_756 ?
Zn1 N1 2.206(4) . ?
Zn1 N3 2.125(4) . ?
Zn1 N4 2.211(5) . ?
Zn1 N5 2.208(4) . ?
Zn1 N7 2.122(4) . ?
Zn1 N8 2.240(4) . ?
N1 C5 1.336(7) . ?
N1 C1 1.356(7) . ?
N2 N3 1.354(6) . ?
N2 C5 1.394(7) . ?
N3 C6 1.290(7) . ?
N4 C11 1.332(7) . ?
N4 C7 1.357(7) . ?
N5 C16 1.344(7) . ?
N5 C12 1.354(7) . ?
N6 N7 1.363(6) . ?
N6 C16 1.380(7) . ?
N7 C17 1.281(7) . ?
N8 C22 1.331(7) . ?
N8 C18 1.354(7) . ?
C1 C2 1.382(8) . ?
C1 C1 1.494(10) 2_656 ?
C2 C3 1.385(8) . ?
C3 C4 1.383(8) . ?
C4 C5 1.406(7) . ?
C6 C7 1.458(8) . ?
C7 C8 1.382(8) . ?
C8 C9 1.404(10) . ?
C9 C10 1.386(10) . ?
C10 C11 1.391(9) . ?
C12 C13 1.380(7) . ?
C12 C12 1.496(10) 2_656 ?
C13 C14 1.401(8) . ?
C14 C15 1.365(8) . ?
C15 C16 1.398(7) . ?
C17 C18 1.463(8) . ?
C18 C19 1.388(8) . ?
C19 C20 1.392(9) . ?
C20 C21 1.376(9) . ?
C21 C22 1.386(9) . ?
