# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_P4_ZnInetwork_100K
_database_code_depnum_ccdc_archive 'CCDC 1440074'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_sum            'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_weight         1615.7

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.5194(6)
_cell_length_b                   30.015(3)
_cell_length_c                   12.7207(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.015(4)
_cell_angle_gamma                90
_cell_volume                     2483.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9820
_cell_measurement_theta_min      2.5925
_cell_measurement_theta_max      26.2535

_exptl_crystal_description       Columnar
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.158
_exptl_crystal_F_000             1494
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.238
_shelx_estimated_absorpt_T_min   0.650
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.536515
_exptl_absorpt_correction_T_max  0.745373
_exptl_absorpt_process_details   'twinabs 2012/1'
_exptl_absorpt_special_details   
;
The crystal under investigation was found to be non-merohedrally twinned.
The orientation matrices for the two components were identified using the
 program Cell_Now, with two components being related by a 180 degree rotation
 around the real and reciprocal axis a. The two components were integrated
using SAINT, resulting in the following statistics :

Statistics for singles of twin component  1
 -------------------------------------------

 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -13.7  0.0980   0.701 - 1.235   0.908 - 1.091   0.628    4974    3067
    2   13.6  0.0955   0.854 - 1.129   0.900 - 1.167   0.616    8128    4991
    3  -13.7  0.0822   0.584 - 0.788   0.925 - 1.167   0.619    4707    3178
    4  -13.7  0.0724   0.540 - 0.603   0.870 - 1.112   0.617    4043    2926
    5  -13.7  0.0755   0.559 - 0.679   0.872 - 1.151   0.665    4834    3178
    6   13.7  0.0999   0.631 - 1.468   0.898 - 1.167   0.635    7123    4255
    7  -13.7  0.0765   0.505 - 0.723   0.889 - 1.136   0.639    4814    3350

   All scans  0.0878   0.505 - 1.468   0.870 - 1.167   0.631   38623   24945


 Statistics for singles of twin component  2
 -------------------------------------------

 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -13.7  0.1873   0.572 - 0.947   0.917 - 1.136   0.628    4924    2064
    2   13.6  0.1806   0.663 - 0.887   0.921 - 1.208   0.616    8149    3483
    3  -13.7  0.1534   0.518 - 0.668   0.938 - 1.208   0.619    4664    2235
    4  -13.7  0.1373   0.465 - 0.516   0.874 - 1.155   0.617    4076    2098
    5  -13.7  0.1382   0.468 - 0.575   0.879 - 1.185   0.665    4827    2325
    6   13.7  0.1846   0.556 - 1.085   0.913 - 1.208   0.635    7063    2953
    7  -13.7  0.1509   0.459 - 0.658   0.896 - 1.154   0.639    4819    2370

   All scans  0.1655   0.459 - 1.085   0.874 - 1.208   0.631   38522   17528

The exact twin matrix identified by the integration program was found to be
(1.00005 -0.00057  0.07137/ -0.01300 -0.99999  0.00531/-0.00154 -0.00104
-1.00005).

The data were corrected for absortpion using twinabs, and the structure was
solved using direct methods with all components. The structure was refined
using the hkl 5 routine with all reflections of component 1, resulting BASF
value of 0.22058.

The Rint value given is for all reflections and is based on agreement between
 observed single and composite intensities and those calculated from refined
unique intensities and twin fractions (TWINABS (Sheldrick, 2012))
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'KAPPA APEX2 QUAZAR Mo, Bruker'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5189
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.357
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5189
_reflns_number_gt                4156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 v2011 .2-0 (Bruker)'
_computing_cell_refinement       'SAINT V8.34A (Bruker)'
_computing_data_reduction        'SAINT V8.34A (Bruker)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0326P)²+11.0197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5189
_refine_ls_number_parameters     285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0932
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
P1 P 0.823(2) 0.7500 -0.1002(11) 0.051(3) Uani 0.2701(10) 2 d S T P . .
P2 P -0.105(2) 0.7500 0.7386(13) 0.073(4) Uani 0.2701(10) 2 d S T P . .
P3 P 0.0878(18) 0.7133(4) 0.8553(10) 0.080(4) Uani 0.2701(10) 1 d . . P . .
C1 C 0.9425(10) 0.6833(2) 0.1891(6) 0.0265(15) Uani 1 1 d . . . . .
H1 H 1.0055 0.6902 0.1259 0.032 Uiso 1 1 calc R U . . .
C2 C 0.7701(10) 0.6570(2) 0.1831(6) 0.0256(15) Uani 1 1 d . . . . .
H2 H 0.7156 0.6459 0.1169 0.031 Uiso 1 1 calc R U . . .
C3 C 0.6754(9) 0.6465(2) 0.2747(5) 0.0220(14) Uani 1 1 d . . . . .
C4 C 0.7630(11) 0.6633(2) 0.3697(5) 0.0265(15) Uani 1 1 d . . . . .
H4 H 0.7034 0.6569 0.4341 0.032 Uiso 1 1 calc R U . . .
C5 C 0.9380(11) 0.6893(2) 0.3687(6) 0.0287(16) Uani 1 1 d . . . . .
H5 H 0.9980 0.7003 0.4339 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4842(10) 0.6207(2) 0.2727(5) 0.0221(14) Uani 1 1 d . . . . .
C7 C -0.1842(11) 0.5490(2) -0.0245(5) 0.0277(16) Uani 1 1 d . . . . .
H7 H -0.3165 0.5355 -0.0279 0.033 Uiso 1 1 calc R U . . .
C8 C -0.0793(11) 0.5546(2) 0.0728(5) 0.0258(16) Uani 1 1 d . . . . .
H8 H -0.1387 0.5453 0.1352 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1142(10) 0.5742(2) 0.0783(5) 0.0228(15) Uani 1 1 d . . . . .
C10 C 0.2008(11) 0.5849(2) -0.0159(6) 0.0300(17) Uani 1 1 d . . . . .
H10 H 0.3367 0.5964 -0.0154 0.036 Uiso 1 1 calc R U . . .
C11 C 0.0865(11) 0.5785(3) -0.1091(6) 0.0323(17) Uani 1 1 d . . . . .
H11 H 0.1459 0.5862 -0.1727 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2192(10) 0.5857(2) 0.1816(5) 0.0245(15) Uani 1 1 d . . . . .
C13 C 0.0287(10) 0.6100(2) 0.6249(5) 0.0258(15) Uani 1 1 d . . . . .
H13 H 0.0508 0.6299 0.6825 0.031 Uiso 1 1 calc R U . . .
C14 C 0.1509(11) 0.6140(2) 0.5408(5) 0.0242(15) Uani 1 1 d . . . . .
H14 H 0.2598 0.6351 0.5423 0.029 Uiso 1 1 calc R U . . .
C15 C 0.1102(10) 0.5865(2) 0.4541(5) 0.0214(15) Uani 1 1 d . . . . .
C16 C -0.0458(11) 0.5548(2) 0.4571(5) 0.0253(15) Uani 1 1 d . . . . .
H16 H -0.0765 0.5355 0.3988 0.030 Uiso 1 1 calc R U . . .
C17 C -0.1534(11) 0.5519(2) 0.5448(5) 0.0259(16) Uani 1 1 d . . . . .
H17 H -0.2570 0.5298 0.5468 0.031 Uiso 1 1 calc R U . . .
C18 C 0.2187(9) 0.5921(2) 0.3574(5) 0.0206(14) Uani 1 1 d . . . . .
N1 N 1.0261(8) 0.69964(18) 0.2806(5) 0.0261(13) Uani 1 1 d . . . . .
N2 N -0.1044(9) 0.56190(19) -0.1153(4) 0.0264(13) Uani 1 1 d . . . . .
N3 N -0.1206(8) 0.57893(19) 0.6288(4) 0.0252(13) Uani 1 1 d . . . . .
N4 N 0.4009(8) 0.60748(18) 0.1782(4) 0.0234(12) Uani 1 1 d . . . . .
N5 N 0.1237(8) 0.57730(17) 0.2674(4) 0.0218(12) Uani 1 1 d . . . . .
N6 N 0.3980(8) 0.61423(17) 0.3639(4) 0.0224(12) Uani 1 1 d . . . . .
Zn1 Zn 1.24893(17) 0.7500 0.28565(10) 0.0314(3) Uani 1 2 d S T P . .
Zn2 Zn -0.30408(12) 0.57504(3) 0.75376(6) 0.02397(18) Uani 1 1 d . . . . .
I1 I 1.41479(11) 0.7500 0.11232(7) 0.0408(2) Uani 1 2 d S T P . .
I2 I 1.41832(11) 0.7500 0.47240(6) 0.0400(2) Uani 1 2 d S T P . .
I3 I -0.45037(8) 0.65120(2) 0.78899(4) 0.03781(14) Uani 1 1 d . . . . .
I4 I -0.55371(7) 0.50928(2) 0.72554(4) 0.02871(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
P1 P2 2.14(2) 1_654 ?
P1 P3 2.157(16) 4_674 ?
P1 P3 2.157(16) 1_654 ?
P2 P1 2.14(2) 1_456 ?
P2 P3 2.178(19) . ?
P2 P3 2.178(19) 4_575 ?
P3 P1 2.157(16) 1_456 ?
P3 P3 2.21(3) 4_575 ?
C1 N1 1.344(9) . ?
C1 C2 1.371(9) . ?
C2 C3 1.392(9) . ?
C3 C4 1.393(9) . ?
C3 C6 1.467(9) . ?
C4 C5 1.383(10) . ?
C5 N1 1.331(9) . ?
C6 N6 1.339(8) . ?
C6 N4 1.344(8) . ?
C7 N2 1.357(9) . ?
C7 C8 1.382(10) . ?
C8 C9 1.389(9) . ?
C9 C10 1.398(10) . ?
C9 C12 1.479(9) . ?
C10 C11 1.368(10) . ?
C11 N2 1.337(9) . ?
C12 N5 1.318(8) . ?
C12 N4 1.356(8) . ?
C13 N3 1.351(9) . ?
C13 C14 1.383(9) . ?
C14 C15 1.389(9) . ?
C15 C16 1.395(10) . ?
C15 C18 1.471(9) . ?
C16 C17 1.361(10) . ?
C17 N3 1.346(9) . ?
C18 N5 1.339(8) . ?
C18 N6 1.342(8) . ?
N1 Zn1 2.094(5) . ?
N2 Zn2 2.079(6) 1_554 ?
N3 Zn2 2.059(6) . ?
Zn1 N1 2.094(5) 4_575 ?
Zn1 I1 2.5228(15) . ?
Zn1 I2 2.5486(15) . ?
Zn2 N2 2.078(6) 1_556 ?
Zn2 I3 2.5291(9) . ?
Zn2 I4 2.5674(9) . ?

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
P2 P1 P3 61.0(6) 1_654 4_674 ?
P2 P1 P3 61.0(6) 1_654 1_654 ?
P3 P1 P3 61.5(8) 4_674 1_654 ?
P1 P2 P3 60.0(6) 1_456 . ?
P1 P2 P3 60.0(6) 1_456 4_575 ?
P3 P2 P3 60.9(8) . 4_575 ?
P1 P3 P2 59.0(6) 1_456 . ?
P1 P3 P3 59.2(4) 1_456 4_575 ?
P2 P3 P3 59.6(4) . 4_575 ?
N1 C1 C2 122.7(6) . . ?
C1 C2 C3 119.5(7) . . ?
C2 C3 C4 117.8(6) . . ?
C2 C3 C6 122.0(6) . . ?
C4 C3 C6 120.1(6) . . ?
C5 C4 C3 119.0(6) . . ?
N1 C5 C4 122.9(7) . . ?
N6 C6 N4 124.4(6) . . ?
N6 C6 C3 118.0(6) . . ?
N4 C6 C3 117.5(6) . . ?
N2 C7 C8 122.1(7) . . ?
C7 C8 C9 119.3(6) . . ?
C8 C9 C10 118.2(6) . . ?
C8 C9 C12 120.4(6) . . ?
C10 C9 C12 121.3(6) . . ?
C11 C10 C9 118.8(7) . . ?
N2 C11 C10 123.5(6) . . ?
N5 C12 N4 125.7(6) . . ?
N5 C12 C9 118.3(6) . . ?
N4 C12 C9 115.8(6) . . ?
N3 C13 C14 123.0(6) . . ?
C13 C14 C15 118.3(6) . . ?
C14 C15 C16 118.9(6) . . ?
C14 C15 C18 121.3(6) . . ?
C16 C15 C18 119.7(6) . . ?
C17 C16 C15 118.9(6) . . ?
N3 C17 C16 123.4(7) . . ?
N5 C18 N6 124.5(6) . . ?
N5 C18 C15 117.2(6) . . ?
N6 C18 C15 118.2(6) . . ?
C5 N1 C1 118.1(6) . . ?
C5 N1 Zn1 118.8(5) . . ?
C1 N1 Zn1 121.9(5) . . ?
C11 N2 C7 117.8(6) . . ?
C11 N2 Zn2 120.4(5) . 1_554 ?
C7 N2 Zn2 118.7(5) . 1_554 ?
C17 N3 C13 117.4(6) . . ?
C17 N3 Zn2 120.7(5) . . ?
C13 N3 Zn2 121.8(5) . . ?
C6 N4 C12 114.4(5) . . ?
C12 N5 C18 115.3(5) . . ?
C6 N6 C18 115.8(6) . . ?
N1 Zn1 N1 92.4(3) 4_575 . ?
N1 Zn1 I1 108.20(16) 4_575 . ?
N1 Zn1 I1 108.19(16) . . ?
N1 Zn1 I2 106.42(17) 4_575 . ?
N1 Zn1 I2 106.42(17) . . ?
I1 Zn1 I2 129.08(5) . . ?
N3 Zn2 N2 105.3(2) . 1_556 ?
N3 Zn2 I3 109.41(16) . . ?
N2 Zn2 I3 104.61(16) 1_556 . ?
N3 Zn2 I4 109.43(16) . . ?
N2 Zn2 I4 108.76(16) 1_556 . ?
I3 Zn2 I4 118.46(3) . . ?

_refine_diff_density_max         1.208
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.178

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_P4_ZnInetwork_200K
_database_code_depnum_ccdc_archive 'CCDC 1440075'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_sum            'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_weight         1615.7

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.5441(4)
_cell_length_b                   30.1738(18)
_cell_length_c                   12.7487(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.705(3)
_cell_angle_gamma                90
_cell_volume                     2512.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9820
_cell_measurement_theta_min      2.5815
_cell_measurement_theta_max      25.232

_exptl_crystal_description       Columnar
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_F_000             1494
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.178
_shelx_estimated_absorpt_T_min   0.653
_shelx_estimated_absorpt_T_max   0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.557617
_exptl_absorpt_correction_T_max  0.745263
_exptl_absorpt_process_details   'twinabs 2012/1'
_exptl_absorpt_special_details   
;
The crystal under investigation was found to be non-merohedrally twinned.
The orientation matrices for the two components were identified using the
 program Cell_Now, with two components being related by a 180 degree rotation
 around the real and reciprocal axis a. The two components were integrated
using SAINT, resulting in the following statistics :

Statistics for singles of twin component  1
 -------------------------------------------

 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -12.9  0.0821   0.645 - 0.994   0.915 - 1.093   0.600    7127    4186
    2   12.9  0.0816   0.671 - 0.794   0.883 - 1.129   0.610    4492    2709
    3   12.9  0.0755   0.656 - 0.734   0.885 - 1.108   0.605    5430    3517
    4  -12.9  0.0737   0.653 - 0.781   0.883 - 1.128   0.635    4892    2937
    5   12.9  0.0792   0.679 - 0.807   0.882 - 1.025   0.624    4765    2847
    6   12.8  0.0820   0.783 - 0.950   0.950 - 1.129   0.596    8223    4836
    7  -12.9  0.0870   0.900 - 1.011   0.953 - 1.129   0.618    5730    3292

   All scans  0.0804   0.645 - 1.011   0.882 - 1.129   0.613   40659   24324


 Statistics for singles of twin component  2
 -------------------------------------------

 Scan 2-theta  R(int)  Incid. factors  Diffr. factors    K     Total I>2sig(I)
    1  -12.9  0.1812   0.570 - 0.876   0.925 - 1.160   0.600    7120    2725
    2   12.9  0.1802   0.583 - 0.696   0.886 - 1.179   0.610    4472    1784
    3   12.9  0.1552   0.561 - 0.663   0.886 - 1.118   0.605    5468    2238
    4  -12.9  0.1582   0.558 - 0.725   0.885 - 1.177   0.635    4912    1886
    5   12.9  0.1667   0.571 - 0.758   0.885 - 1.088   0.624    4754    1822
    6   12.8  0.1789   0.637 - 0.802   0.945 - 1.180   0.596    8210    3158
    7  -12.9  0.1850   0.663 - 0.857   0.939 - 1.180   0.618    5660    2131

   All scans  0.1731   0.558 - 0.876   0.885 - 1.180   0.613   40596   15744

The exact twin matrix identified by the integration program was found to be
(1.00007 -0.00048  0.06580/-0.01099 -0.99999  0.00547/-0.00210 -0.00104
-1.00007).

The data were corrected for absortpion using twinabs, and the structure was
solved using direct methods with all components. The structure was refined
using the hkl 5 routine with all reflections of component 1, resulting BASF
value of 0.18655.

The Rint value given is for all reflections and is based on agreement between
 observed single and composite intensities and those calculated from refined
unique intensities and twin fractions (TWINABS (Sheldrick, 2012))
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'KAPPA APEX2 QUAZAR Mo, Bruker'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4862
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.350
_diffrn_reflns_theta_max         25.727
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4862
_reflns_number_gt                3593
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 v2011 .2-0 (Bruker)'
_computing_cell_refinement       'SAINT V8.34A (Bruker)'
_computing_data_reduction        'SAINT V8.34A (Bruker)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+9.1015P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4862
_refine_ls_number_parameters     285
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
P1 P 0.826(3) 0.7500 -0.1089(14) 0.096(5) Uani 0.2701(10) 2 d S T P . .
P2 P -0.106(4) 0.7500 0.7311(17) 0.137(7) Uani 0.2701(10) 2 d S T P . .
P3 P 0.084(2) 0.7139(5) 0.8479(14) 0.140(6) Uani 0.2701(10) 1 d . . P . .
C1 C 0.9332(10) 0.6837(2) 0.1865(6) 0.0446(17) Uani 1 1 d . . . . .
H1 H 0.9950 0.6910 0.1234 0.054 Uiso 1 1 calc R U . . .
C2 C 0.7613(10) 0.6571(2) 0.1815(6) 0.0406(16) Uani 1 1 d . . . . .
H2 H 0.7064 0.6461 0.1158 0.049 Uiso 1 1 calc R U . . .
C3 C 0.6705(9) 0.6467(2) 0.2724(5) 0.0350(15) Uani 1 1 d . . . . .
C4 C 0.7552(10) 0.6630(2) 0.3680(6) 0.0376(16) Uani 1 1 d . . . . .
H4 H 0.6963 0.6562 0.4323 0.045 Uiso 1 1 calc R U . . .
C5 C 0.9265(10) 0.6893(2) 0.3661(6) 0.0443(17) Uani 1 1 d . . . . .
H5 H 0.9842 0.7007 0.4309 0.053 Uiso 1 1 calc R U . . .
C6 C 0.4770(9) 0.6211(2) 0.2721(5) 0.0338(14) Uani 1 1 d . . . . .
C7 C -0.1849(11) 0.5497(2) -0.0252(5) 0.0440(18) Uani 1 1 d . . . . .
H7 H -0.3166 0.5363 -0.0280 0.053 Uiso 1 1 calc R U . . .
C8 C -0.0805(10) 0.5551(2) 0.0707(5) 0.0408(17) Uani 1 1 d . . . . .
H8 H -0.1390 0.5451 0.1328 0.049 Uiso 1 1 calc R U . . .
C9 C 0.1095(9) 0.5750(2) 0.0770(5) 0.0351(15) Uani 1 1 d . . . . .
C10 C 0.1948(11) 0.5860(3) -0.0160(5) 0.050(2) Uani 1 1 d . . . . .
H10 H 0.3292 0.5979 -0.0154 0.060 Uiso 1 1 calc R U . . .
C11 C 0.0820(11) 0.5793(3) -0.1092(5) 0.050(2) Uani 1 1 d . . . . .
H11 H 0.1419 0.5870 -0.1726 0.061 Uiso 1 1 calc R U . . .
C12 C 0.2153(9) 0.5866(2) 0.1798(5) 0.0309(14) Uani 1 1 d . . . . .
C13 C 0.0253(10) 0.6091(2) 0.6237(5) 0.0393(16) Uani 1 1 d . . . . .
H13 H 0.0480 0.6289 0.6814 0.047 Uiso 1 1 calc R U . . .
C14 C 0.1464(10) 0.6133(2) 0.5395(5) 0.0362(16) Uani 1 1 d . . . . .
H14 H 0.2546 0.6343 0.5408 0.043 Uiso 1 1 calc R U . . .
C15 C 0.1064(9) 0.5861(2) 0.4529(5) 0.0312(14) Uani 1 1 d . . . . .
C16 C -0.0484(10) 0.5552(2) 0.4560(5) 0.0387(16) Uani 1 1 d . . . . .
H16 H -0.0801 0.5363 0.3975 0.046 Uiso 1 1 calc R U . . .
C17 C -0.1561(11) 0.5520(2) 0.5446(5) 0.0411(17) Uani 1 1 d . . . . .
H17 H -0.2591 0.5299 0.5467 0.049 Uiso 1 1 calc R U . . .
C18 C 0.2151(9) 0.5926(2) 0.3556(5) 0.0327(15) Uani 1 1 d . . . . .
N1 N 1.0155(8) 0.69953(17) 0.2788(5) 0.0424(14) Uani 1 1 d . . . . .
N2 N -0.1069(8) 0.5627(2) -0.1156(4) 0.0401(14) Uani 1 1 d . . . . .
N3 N -0.1234(8) 0.57845(18) 0.6280(4) 0.0362(13) Uani 1 1 d . . . . .
N4 N 0.3935(8) 0.60772(17) 0.1765(4) 0.0350(12) Uani 1 1 d . . . . .
N5 N 0.1203(7) 0.57772(17) 0.2669(4) 0.0334(12) Uani 1 1 d . . . . .
N6 N 0.3921(8) 0.61429(17) 0.3627(4) 0.0356(13) Uani 1 1 d . . . . .
Zn1 Zn 1.23727(17) 0.7500 0.28321(11) 0.0487(3) Uani 1 2 d S T P . .
Zn2 Zn -0.30484(11) 0.57496(3) 0.75341(6) 0.0380(2) Uani 1 1 d . . . . .
I1 I 1.40404(12) 0.7500 0.11053(7) 0.0666(2) Uani 1 2 d S T P . .
I2 I 1.40644(12) 0.7500 0.46862(7) 0.0650(2) Uani 1 2 d S T P . .
I3 I -0.45175(8) 0.65072(2) 0.78577(5) 0.06492(18) Uani 1 1 d . . . . .
I4 I -0.55060(7) 0.50917(2) 0.72808(4) 0.04764(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
P1 P3 2.113(19) 4_674 ?
P1 P3 2.113(19) 1_654 ?
P1 P2 2.12(3) 1_654 ?
P2 P1 2.12(3) 1_456 ?
P2 P3 2.17(3) . ?
P2 P3 2.17(3) 4_575 ?
P3 P1 2.113(19) 1_456 ?
P3 P3 2.18(3) 4_575 ?
C1 N1 1.350(9) . ?
C1 C2 1.380(9) . ?
C2 C3 1.372(9) . ?
C3 C4 1.396(9) . ?
C3 C6 1.483(8) . ?
C4 C5 1.374(9) . ?
C5 N1 1.326(9) . ?
C6 N6 1.330(8) . ?
C6 N4 1.364(8) . ?
C7 N2 1.349(8) . ?
C7 C8 1.371(9) . ?
C8 C9 1.379(9) . ?
C9 C10 1.384(9) . ?
C9 C12 1.483(9) . ?
C10 C11 1.372(9) . ?
C11 N2 1.332(9) . ?
C12 N4 1.332(8) . ?
C12 N5 1.334(8) . ?
C13 N3 1.347(8) . ?
C13 C14 1.381(9) . ?
C14 C15 1.386(9) . ?
C15 C16 1.380(9) . ?
C15 C18 1.482(9) . ?
C16 C17 1.374(9) . ?
C17 N3 1.335(8) . ?
C18 N6 1.328(8) . ?
C18 N5 1.332(7) . ?
N1 Zn1 2.102(5) . ?
N2 Zn2 2.080(5) 1_554 ?
N3 Zn2 2.055(5) . ?
Zn1 N1 2.102(5) 4_575 ?
Zn1 I1 2.5194(16) . ?
Zn1 I2 2.5446(16) . ?
Zn2 N2 2.080(5) 1_556 ?
Zn2 I3 2.5242(10) . ?
Zn2 I4 2.5621(9) . ?

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
P3 P1 P3 62.0(11) 4_674 1_654 ?
P3 P1 P2 61.7(8) 4_674 1_654 ?
P3 P1 P2 61.7(9) 1_654 1_654 ?
P1 P2 P3 59.0(8) 1_456 . ?
P1 P2 P3 59.0(8) 1_456 4_575 ?
P3 P2 P3 60.2(10) . 4_575 ?
P1 P3 P2 59.2(8) 1_456 . ?
P1 P3 P3 59.0(5) 1_456 4_575 ?
P2 P3 P3 59.9(5) . 4_575 ?
N1 C1 C2 121.6(7) . . ?
C3 C2 C1 119.4(7) . . ?
C2 C3 C4 119.1(6) . . ?
C2 C3 C6 122.2(6) . . ?
C4 C3 C6 118.5(6) . . ?
C5 C4 C3 117.9(6) . . ?
N1 C5 C4 123.5(7) . . ?
N6 C6 N4 124.4(6) . . ?
N6 C6 C3 118.9(6) . . ?
N4 C6 C3 116.7(5) . . ?
N2 C7 C8 122.2(7) . . ?
C7 C8 C9 120.0(6) . . ?
C8 C9 C10 117.8(6) . . ?
C8 C9 C12 121.5(6) . . ?
C10 C9 C12 120.6(6) . . ?
C11 C10 C9 118.9(7) . . ?
N2 C11 C10 123.6(6) . . ?
N4 C12 N5 125.3(6) . . ?
N4 C12 C9 116.4(5) . . ?
N5 C12 C9 118.1(5) . . ?
N3 C13 C14 123.1(6) . . ?
C13 C14 C15 118.5(6) . . ?
C16 C15 C14 118.6(6) . . ?
C16 C15 C18 120.4(6) . . ?
C14 C15 C18 120.9(6) . . ?
C17 C16 C15 119.2(6) . . ?
N3 C17 C16 123.3(6) . . ?
N6 C18 N5 125.5(6) . . ?
N6 C18 C15 118.1(5) . . ?
N5 C18 C15 116.4(5) . . ?
C5 N1 C1 118.5(6) . . ?
C5 N1 Zn1 119.1(5) . . ?
C1 N1 Zn1 121.1(5) . . ?
C11 N2 C7 117.3(6) . . ?
C11 N2 Zn2 120.6(4) . 1_554 ?
C7 N2 Zn2 119.2(5) . 1_554 ?
C17 N3 C13 117.2(5) . . ?
C17 N3 Zn2 121.2(4) . . ?
C13 N3 Zn2 121.5(4) . . ?
C12 N4 C6 114.5(5) . . ?
C18 N5 C12 115.0(5) . . ?
C18 N6 C6 115.3(5) . . ?
N1 Zn1 N1 92.9(3) 4_575 . ?
N1 Zn1 I1 108.30(18) 4_575 . ?
N1 Zn1 I1 108.30(18) . . ?
N1 Zn1 I2 106.44(17) 4_575 . ?
N1 Zn1 I2 106.44(17) . . ?
I1 Zn1 I2 128.66(5) . . ?
N3 Zn2 N2 105.8(2) . 1_556 ?
N3 Zn2 I3 109.03(15) . . ?
N2 Zn2 I3 104.70(16) 1_556 . ?
N3 Zn2 I4 109.35(15) . . ?
N2 Zn2 I4 108.48(17) 1_556 . ?
I3 Zn2 I4 118.67(3) . . ?

_refine_diff_density_max         0.756
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.134

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_P4_network_P21_m
_database_code_depnum_ccdc_archive 'CCDC 1440077'
_audit_update_record             
;
2016-02-03 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C36 I6 N12 P3.76 Zn3'
_chemical_formula_weight         1674.50
_chemical_melting_point          ?


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 'International Tables for Crystallography, Vol. C'
I I -0.5797 1.5647 'International Tables for Crystallography, Vol. C'
N N 0.0049 0.0027 'International Tables for Crystallography, Vol. C'
P P 0.0887 0.0799 'International Tables for Crystallography, Vol. C'
Zn Zn 0.3193 1.2372 'International Tables for Crystallography, Vol. C'

#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_Int_Tables_number      11

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y+1/2,-z
3 -x,-y,-z
4 x,-y+1/2,z

_cell_length_a                   12.7069(3)
_cell_length_b                   30.5552(8)
_cell_length_c                   6.5079(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.488(2)
_cell_angle_gamma                90
_cell_volume                     2515.2(1)
_cell_formula_units_Z            2
_cell_measurement_temperature    134(2)
_cell_special_details            ?
_cell_measurement_reflns_used    10534
_cell_measurement_theta_min      2.5026
_cell_measurement_theta_max      33.9962
_exptl_crystal_density_diffrn    2.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484.70
_exptl_absorpt_coefficient_mu    4.140
_pd_spec_mounting                capillary
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_char_colour                  'pale green'


#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

_diffrn_ambient_temperature      134(2)
_diffrn_source                   synchrotron
_diffrn_source_type              'SPring-8 BL15XU'
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  IP
_diffrn_detector                 ?
_diffrn_detector_type            ?
_pd_meas_scan_method             step
_pd_meas_special_details         
; ?
;

_diffrn_radiation_wavelength     0.652970
_diffrn_radiation_monochromator  ?
_pd_meas_number_of_points        10534
_pd_meas_2theta_range_min        2.5026
_pd_meas_2theta_range_max        33.9962
_pd_meas_2theta_range_inc        0.0030

#===============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_calc_method                  'Rietveld Refinement'

_pd_proc_ls_profile_function     'split pseudo-Voigt function'
_pd_proc_ls_background_function  'Legendre polynomials'
_pd_proc_ls_pref_orient_corr     
; ?
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)

_pd_proc_ls_prof_R_factor        0.04340
_pd_proc_ls_prof_wR_factor       0.05067
_pd_proc_ls_prof_wR_expected     0.31218
_refine_ls_R_I_factor            0.04738
_refine_ls_R_Fsqd_factor         0.01783
_refine_ls_R_factor_all          0.01782

_refine_special_details          
; ?
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/yi
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     270
_refine_ls_number_restraints     136
_refine_ls_number_constraints    36
_refine_ls_goodness_of_fit_all   0.1623
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          1.0E-6
_refine_ls_shift/su_mean         ?
_refine_diff_density_max         0.0
_refine_diff_density_min         0.0


_pd_proc_2theta_range_min        2.5026
_pd_proc_2theta_range_max        33.9962
_pd_proc_2theta_range_inc        0.0030
_pd_proc_wavelength              0.65297


_computing_data_collection       ?
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    DASH
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
N1 1.124(3) 0.616(1) 0.094(6) 1 4 f Uiso 0.02647 N
C2 1.136(4) 0.591(2) 0.284(8) 1 4 f Uiso 0.02647 C
C3 1.213(5) 0.623(2) 0.009(8) 1 4 f Uiso 0.02647 C
C4 1.050(4) 0.584(2) 0.394(8) 1 4 f Uiso 0.02647 C
N5 1.230(4) 0.576(1) 0.372(6) 1 4 f Uiso 0.02647 N
C6 1.204(4) 0.654(1) -0.184(8) 1 4 f Uiso 0.02647 C
N7 1.308(3) 0.610(1) 0.089(6) 1 4 f Uiso 0.02647 N
C8 0.956(4) 0.611(2) 0.360(7) 1 4 f Uiso 0.02647 C
C9 1.056(4) 0.553(2) 0.552(7) 1 4 f Uiso 0.02647 C
C10 1.311(4) 0.586(2) 0.287(8) 1 4 f Uiso 0.02647 C
C11 1.112(4) 0.667(2) -0.260(9) 1 4 f Uiso 0.02647 C
C12 1.292(4) 0.668(2) -0.281(8) 1 4 f Uiso 0.02647 C
C13 0.871(4) 0.602(2) 0.492(8) 1 4 f Uiso 0.02647 C
C14 0.960(4) 0.549(2) 0.665(8) 1 4 f Uiso 0.02647 C
C15 1.408(4) 0.577(2) 0.393(8) 1 4 f Uiso 0.02647 C
C16 1.107(4) 0.694(2) -0.443(8) 1 4 f Uiso 0.02647 C
C17 1.278(4) 0.694(1) -0.465(9) 1 4 f Uiso 0.02647 C
N18 0.876(3) 0.572(1) 0.629(6) 1 4 f Uiso 0.02647 N
C19 1.420(4) 0.556(2) 0.570(7) 1 4 f Uiso 0.02647 C
C20 1.499(4) 0.591(2) 0.303(7) 1 4 f Uiso 0.02647 C
N21 1.188(3) 0.706(1) -0.545(6) 1 4 f Uiso 0.02647 N
Zn22 0.7429(5) 0.5712(2) 0.7943(9) 1 4 f Uiso 0.02647 Zn
C23 1.529(4) 0.549(2) 0.679(7) 1 4 f Uiso 0.02647 C
C24 1.601(4) 0.581(2) 0.409(8) 1 4 f Uiso 0.02647 C
Zn25 1.178(1) 0.75 -0.754(3) 1 2 e Uiso 0.02647 Zn
I26 0.7710(3) 0.5085(1) 1.0518(6) 1 4 f Uiso 0.02647 I
I27 0.7080(3) 0.6473(1) 0.9534(5) 1 4 f Uiso 0.02647 I
N28 1.613(3) 0.559(1) 0.603(6) 1 4 f Uiso 0.02647 N
I29 0.9930(4) 0.7445(4) -0.9085(8) 0.5 4 f Uiso 0.02647 I
I30 1.3498(4) 0.7577(3) -0.9162(8) 0.5 4 f Uiso 0.02647 I
P31 0.743(2) -0.263(1) -0.415(4) 0.47 4 f Uiso 0.02647 P
P32 0.580(3) -0.25 -0.332(7) 0.94 2 e Uiso 0.02647 P
P33 0.603(2) -0.297(1) -0.569(5) 0.47 4 f Uiso 0.02647 P
P34 0.627(3) -0.2269(9) -0.629(5) 0.47 4 f Uiso 0.02647 P

#===============================================================================

#10. GEOMETRICAL PARAMETERS

_geom_special_details            ?

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 C3 1.32(5) . 1_555 ?
N1 C2 1.44(5) . 1_555 ?
N1 N7 2.34(5) . 1_555 ?
N1 C4 2.45(7) . 1_555 ?
N1 C6 2.45(6) . 1_555 ?
N1 N5 2.46(5) . 1_555 ?
N1 C10 2.73(7) . 1_555 ?
N1 C11 2.78(7) . 1_555 ?
N1 C8 2.88(6) . 1_555 ?
N1 N21 3.66(5) . 1_556 ?
N1 C9 3.71(7) . 1_555 ?
N1 C12 3.74(7) . 1_555 ?
C2 N5 1.35(5) . 1_555 ?
C2 C4 1.38(6) . 1_555 ?
C2 N1 1.44(5) . 1_555 ?
C2 C10 2.22(6) . 1_555 ?
C2 C3 2.33(6) . 1_555 ?
C2 C9 2.40(7) . 1_555 ?
C2 C8 2.46(7) . 1_555 ?
C2 N7 2.69(6) . 1_555 ?
C2 C15 3.48(7) . 1_555 ?
C2 C16 3.66(6) . 1_556 ?
C2 N21 3.72(6) . 1_556 ?
C2 C14 3.73(7) . 1_555 ?
C2 C13 3.76(7) . 1_555 ?
C2 C6 3.77(7) . 1_555 ?
C3 N1 1.32(5) . 1_555 ?
C3 N7 1.32(5) . 1_555 ?
C3 C6 1.58(5) . 1_555 ?
C3 C2 2.33(6) . 1_555 ?
C3 C10 2.37(6) . 1_555 ?
C3 C11 2.48(8) . 1_555 ?
C3 C12 2.61(8) . 1_555 ?
C3 N5 2.75(6) . 1_555 ?
C3 C4 3.60(7) . 1_555 ?
C3 C15 3.62(7) . 1_555 ?
C4 C2 1.38(6) . 1_555 ?
C4 C9 1.39(5) . 1_555 ?
C4 C8 1.45(6) . 1_555 ?
C4 N5 2.31(7) . 1_555 ?
C4 C14 2.44(7) . 1_555 ?
C4 N1 2.45(7) . 1_555 ?
C4 C13 2.48(7) . 1_555 ?
C4 N18 2.84(7) . 1_555 ?
C4 C11 3.44(6) . 1_556 ?
C4 C10 3.45(7) . 1_555 ?
C4 C16 3.59(6) . 1_556 ?
C4 C3 3.60(7) . 1_555 ?
N5 C10 1.25(5) . 1_555 ?
N5 C2 1.35(5) . 1_555 ?
N5 C15 2.26(6) . 1_555 ?
N5 C4 2.31(7) . 1_555 ?
N5 N7 2.41(5) . 1_555 ?
N5 N1 2.46(5) . 1_555 ?
N5 C19 2.69(7) . 1_555 ?
N5 C9 2.69(6) . 1_555 ?
N5 C3 2.75(6) . 1_555 ?
N5 C20 3.52(6) . 1_555 ?
N5 C8 3.63(7) . 1_555 ?
N5 C12 3.64(6) . 1_556 ?
N5 C17 3.78(6) . 1_556 ?
N5 C6 3.79(6) . 1_556 ?
C6 C11 1.29(6) . 1_555 ?
C6 C12 1.40(5) . 1_555 ?
C6 C3 1.58(5) . 1_555 ?
C6 C16 2.34(6) . 1_555 ?
C6 N1 2.45(6) . 1_555 ?
C6 C17 2.46(7) . 1_555 ?
C6 N7 2.50(7) . 1_555 ?
C6 N21 2.82(7) . 1_555 ?
C6 I30 3.62(5) . 4_566 ?
C6 C2 3.77(7) . 1_555 ?
C6 N5 3.79(6) . 1_554 ?
N7 C3 1.32(5) . 1_555 ?
N7 C10 1.48(5) . 1_555 ?
N7 N1 2.34(5) . 1_555 ?
N7 N5 2.41(5) . 1_555 ?
N7 C15 2.46(7) . 1_555 ?
N7 C6 2.50(7) . 1_555 ?
N7 C2 2.69(6) . 1_555 ?
N7 C20 2.74(6) . 1_555 ?
N7 C12 2.97(7) . 1_555 ?
N7 C11 3.65(7) . 1_555 ?
N7 C19 3.70(7) . 1_555 ?
C8 C4 1.45(6) . 1_555 ?
C8 C13 1.46(5) . 1_555 ?
C8 N18 2.42(5) . 1_555 ?
C8 C9 2.43(7) . 1_555 ?
C8 C2 2.46(7) . 1_555 ?
C8 C14 2.73(6) . 1_555 ?
C8 N1 2.88(6) . 1_555 ?
C8 C16 3.38(6) . 1_556 ?
C8 C11 3.48(7) . 1_556 ?
C8 N5 3.63(7) . 1_555 ?
C9 C4 1.39(5) . 1_555 ?
C9 C14 1.49(5) . 1_555 ?
C9 C2 2.40(7) . 1_555 ?
C9 C8 2.43(7) . 1_555 ?
C9 N18 2.45(6) . 1_555 ?
C9 N5 2.69(6) . 1_555 ?
C9 C13 2.78(6) . 1_555 ?
C9 N1 3.71(7) . 1_555 ?
C9 C11 3.74(7) . 1_556 ?
C10 N5 1.25(5) . 1_555 ?
C10 C15 1.38(6) . 1_555 ?
C10 N7 1.48(5) . 1_555 ?
C10 C2 2.22(6) . 1_555 ?
C10 C3 2.37(6) . 1_555 ?
C10 C19 2.38(7) . 1_555 ?
C10 C20 2.39(7) . 1_555 ?
C10 N1 2.73(7) . 1_555 ?
C10 C4 3.45(7) . 1_555 ?
C10 C24 3.70(7) . 1_555 ?
C10 C17 3.70(6) . 1_556 ?
C10 C23 3.76(7) . 1_555 ?
C10 C12 3.79(6) . 1_556 ?
C11 C6 1.29(6) . 1_555 ?
C11 C16 1.45(6) . 1_555 ?
C11 C12 2.31(6) . 1_555 ?
C11 N21 2.47(6) . 1_555 ?
C11 C3 2.48(8) . 1_555 ?
C11 C17 2.73(6) . 1_555 ?
C11 N1 2.78(7) . 1_555 ?
C11 C4 3.44(6) . 1_554 ?
C11 C8 3.48(7) . 1_554 ?
C11 N7 3.65(7) . 1_555 ?
C11 I29 3.71(5) . 1_556 ?
C11 C9 3.74(7) . 1_554 ?
C12 C6 1.40(5) . 1_555 ?
C12 C17 1.43(6) . 1_555 ?
C12 C11 2.31(6) . 1_555 ?
C12 N21 2.37(6) . 1_555 ?
C12 C16 2.61(6) . 1_555 ?
C12 C3 2.61(8) . 1_555 ?
C12 N7 2.97(7) . 1_555 ?
C12 I30 3.32(4) . 4_566 ?
C12 N5 3.64(6) . 1_554 ?
C12 I30 3.66(4) . 1_556 ?
C12 N1 3.74(7) . 1_555 ?
C12 C10 3.79(6) . 1_554 ?
C13 N18 1.29(5) . 1_555 ?
C13 C8 1.46(5) . 1_555 ?
C13 C14 2.22(6) . 1_555 ?
C13 C4 2.48(7) . 1_555 ?
C13 C9 2.78(6) . 1_555 ?
C13 Zn22 2.84(6) . 1_555 ?
C13 C24 3.49(7) . 1_455 ?
C13 N28 3.68(7) . 1_455 ?
C13 C2 3.76(7) . 1_555 ?
C14 N18 1.28(5) . 1_555 ?
C14 C9 1.49(5) . 1_555 ?
C14 C13 2.22(6) . 1_555 ?
C14 C4 2.44(7) . 1_555 ?
C14 C8 2.73(6) . 1_555 ?
C14 Zn22 3.04(6) . 1_555 ?
C14 C2 3.73(7) . 1_555 ?
C15 C19 1.32(5) . 1_555 ?
C15 C10 1.38(6) . 1_555 ?
C15 C20 1.41(6) . 1_555 ?
C15 N5 2.26(6) . 1_555 ?
C15 C24 2.45(7) . 1_555 ?
C15 N7 2.46(7) . 1_555 ?
C15 C23 2.46(7) . 1_555 ?
C15 N28 2.87(7) . 1_555 ?
C15 C2 3.48(7) . 1_555 ?
C15 C3 3.62(7) . 1_555 ?
C16 N21 1.33(4) . 1_555 ?
C16 C11 1.45(6) . 1_555 ?
C16 C17 2.19(5) . 1_555 ?
C16 C6 2.34(6) . 1_555 ?
C16 C12 2.61(6) . 1_555 ?
C16 Zn25 2.86(6) . 1_555 ?
C16 N21 3.30(5) . 4_565 ?
C16 C8 3.38(6) . 1_554 ?
C16 C16 3.39(9) . 4_565 ?
C16 I29 3.57(5) . 1_555 ?
C16 C4 3.59(6) . 1_554 ?
C16 C2 3.66(6) . 1_554 ?
C16 I29 3.73(5) . 4_565 ?
C17 N21 1.26(5) . 1_555 ?
C17 C12 1.43(6) . 1_555 ?
C17 C16 2.19(5) . 1_555 ?
C17 C6 2.46(7) . 1_555 ?
C17 C11 2.73(6) . 1_555 ?
C17 Zn25 2.76(6) . 1_555 ?
C17 N21 3.30(5) . 4_565 ?
C17 C17 3.44(9) . 4_565 ?
C17 I30 3.49(5) . 4_565 ?
C17 C10 3.70(6) . 1_554 ?
C17 I30 3.71(5) . 1_555 ?
C17 N5 3.78(6) . 1_554 ?
N18 C14 1.28(5) . 1_555 ?
N18 C13 1.29(5) . 1_555 ?
N18 Zn22 2.09(4) . 1_555 ?
N18 C8 2.42(5) . 1_555 ?
N18 C9 2.45(6) . 1_555 ?
N18 C4 2.84(7) . 1_555 ?
N18 N28 3.35(5) . 1_455 ?
N18 C24 3.66(7) . 1_455 ?
N18 I26 3.71(4) . 1_555 ?
C19 C15 1.32(5) . 1_555 ?
C19 C23 1.51(5) . 1_555 ?
C19 C20 2.35(6) . 1_555 ?
C19 C10 2.38(7) . 1_555 ?
C19 N28 2.44(5) . 1_555 ?
C19 N5 2.69(7) . 1_555 ?
C19 C24 2.73(7) . 1_555 ?
C19 N7 3.70(7) . 1_555 ?
C20 C15 1.41(6) . 1_555 ?
C20 C24 1.44(5) . 1_555 ?
C20 C19 2.35(6) . 1_555 ?
C20 C10 2.39(7) . 1_555 ?
C20 N28 2.51(5) . 1_555 ?
C20 N7 2.74(6) . 1_555 ?
C20 C23 2.77(6) . 1_555 ?
C20 N5 3.52(6) . 1_555 ?
C20 P33 3.72(6) . 1_666 ?
N21 C17 1.26(5) . 1_555 ?
N21 C16 1.33(4) . 1_555 ?
N21 Zn25 1.91(4) . 1_555 ?
N21 C12 2.37(6) . 1_555 ?
N21 C11 2.47(6) . 1_555 ?
N21 N21 2.70(7) . 4_565 ?
N21 C6 2.82(7) . 1_555 ?
N21 C17 3.30(5) . 4_565 ?
N21 C16 3.30(5) . 4_565 ?
N21 I29 3.47(4) . 1_555 ?
N21 I30 3.50(4) . 4_565 ?
N21 I29 3.59(4) . 4_565 ?
N21 N1 3.66(5) . 1_554 ?
N21 I30 3.67(4) . 1_555 ?
N21 C2 3.72(6) . 1_554 ?
Zn22 N28 2.01(4) . 1_455 ?
Zn22 N18 2.09(4) . 1_555 ?
Zn22 I26 2.549(6) . 1_555 ?
Zn22 I27 2.600(7) . 1_555 ?
Zn22 C13 2.84(6) . 1_555 ?
Zn22 C23 2.84(5) . 1_455 ?
Zn22 C24 2.96(6) . 1_455 ?
Zn22 C14 3.04(6) . 1_555 ?
C23 N28 1.26(5) . 1_555 ?
C23 C19 1.51(5) . 1_555 ?
C23 C24 2.29(7) . 1_555 ?
C23 C15 2.46(7) . 1_555 ?
C23 C20 2.77(6) . 1_555 ?
C23 Zn22 2.84(5) . 1_655 ?
C23 C10 3.76(7) . 1_555 ?
C24 N28 1.42(5) . 1_555 ?
C24 C20 1.44(5) . 1_555 ?
C24 C23 2.29(7) . 1_555 ?
C24 C15 2.45(7) . 1_555 ?
C24 C19 2.73(7) . 1_555 ?
C24 Zn22 2.96(6) . 1_655 ?
C24 C13 3.49(7) . 1_655 ?
C24 N18 3.66(7) . 1_655 ?
C24 C10 3.70(7) . 1_555 ?
C24 P33 3.72(6) . 1_666 ?
Zn25 N21 1.91(4) . 1_555 ?
Zn25 N21 1.91(4) . 4_565 ?
Zn25 I29 2.48(2) . 1_555 ?
Zn25 I29 2.48(2) . 4_565 ?
Zn25 I30 2.52(2) . 1_555 ?
Zn25 I30 2.52(2) . 4_565 ?
Zn25 C17 2.76(6) . 1_555 ?
Zn25 C17 2.76(6) . 4_565 ?
Zn25 C16 2.86(6) . 1_555 ?
Zn25 C16 2.86(6) . 4_565 ?
I26 Zn22 2.549(6) . 1_555 ?
I26 N18 3.71(4) . 1_555 ?
I26 N28 3.73(4) . 1_455 ?
I27 Zn22 2.600(7) . 1_555 ?
I27 N28 3.65(4) . 1_455 ?
I27 P31 3.71(3) . 1_566 ?
N28 C23 1.26(5) . 1_555 ?
N28 C24 1.42(5) . 1_555 ?
N28 Zn22 2.01(4) . 1_655 ?
N28 C19 2.44(5) . 1_555 ?
N28 C20 2.51(5) . 1_555 ?
N28 C15 2.87(7) . 1_555 ?
N28 N18 3.35(5) . 1_655 ?
N28 I27 3.65(4) . 1_655 ?
N28 C13 3.68(7) . 1_655 ?
N28 I26 3.73(4) . 1_655 ?
I29 I29 0.34(3) . 4_565 ?
I29 Zn25 2.48(2) . 1_555 ?
I29 N21 3.47(4) . 1_555 ?
I29 C16 3.57(5) . 1_555 ?
I29 N21 3.59(4) . 4_565 ?
I29 C11 3.71(5) . 1_554 ?
I29 C16 3.73(5) . 4_565 ?
I30 I30 0.47(2) . 4_565 ?
I30 Zn25 2.52(2) . 1_555 ?
I30 C12 3.32(4) . 4_564 ?
I30 C17 3.49(5) . 4_565 ?
I30 N21 3.50(4) . 4_565 ?
I30 C6 3.62(5) . 4_564 ?
I30 C12 3.66(4) . 1_554 ?
I30 N21 3.67(4) . 1_555 ?
I30 C17 3.71(5) . 1_555 ?
P31 P31 0.77(6) . 4_545 ?
P31 P34 1.96(3) . 4_545 ?
P31 P34 2.22(4) . 1_555 ?
P31 P33 2.22(4) . 1_555 ?
P31 P32 2.23(4) . 1_555 ?
P31 P33 2.67(4) . 4_545 ?
P31 I27 3.71(3) . 1_544 ?
P32 P33 2.15(5) . 1_555 ?
P32 P33 2.15(5) . 4_545 ?
P32 P34 2.19(4) . 1_555 ?
P32 P34 2.19(4) . 4_545 ?
P32 P31 2.23(4) . 1_555 ?
P32 P31 2.23(4) . 4_545 ?
P33 P34 0.89(3) . 4_545 ?
P33 P32 2.15(5) . 1_555 ?
P33 P34 2.21(4) . 1_555 ?
P33 P31 2.22(4) . 1_555 ?
P33 P31 2.67(4) . 4_545 ?
P33 P33 2.88(6) . 4_545 ?
P33 C20 3.72(6) . 1_444 ?
P33 C24 3.72(6) . 1_444 ?
P34 P33 0.89(3) . 4_545 ?
P34 P34 1.41(5) . 4_545 ?
P34 P31 1.96(3) . 4_545 ?
P34 P32 2.19(4) . 1_555 ?
P34 P33 2.21(4) . 1_555 ?
P34 P31 2.22(4) . 1_555 ?

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
C3 C4 N1 13(1) 1_555 . 1_555 ?
C3 C4 C2 18(4) 1_555 . 1_555 ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_P4_ZnInetwork_300K
_database_code_depnum_ccdc_archive 'CCDC 1457373'
_audit_update_record             
;
2016-03-03 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_sum            'C36 H24 I6 N12 P1.08 Zn3'
_chemical_formula_weight         1615.7

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.6025(6)
_cell_length_b                   30.199(3)
_cell_length_c                   12.8199(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.491(3)
_cell_angle_gamma                90
_cell_volume                     2556.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.5725
_cell_measurement_theta_max      23.0515

_exptl_crystal_description       Columnar
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_F_000             1494
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.089
_shelx_estimated_absorpt_T_min   0.657
_shelx_estimated_absorpt_T_max   0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5775
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'KAPPA APEX2 QUAZAR Mo, Bruker'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32015
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.349
_diffrn_reflns_theta_max         23.313
_diffrn_reflns_theta_full        23.313
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3751
_reflns_number_gt                2764
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 v2011 .2-0 (Bruker)'
_computing_cell_refinement       'SAINT V8.34A (Bruker)'
_computing_data_reduction        'SAINT V8.34A (Bruker)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  WinGX
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+24.7252P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3751
_refine_ls_number_parameters     285
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1071
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
P1 P -0.331(11) 0.7500 0.151(6) 0.25(3) Uani 0.270(11) 2 d S TU P . .
P2 P -0.384(9) 0.7500 0.312(6) 0.25(3) Uani 0.270(11) 2 d S TU P . .
P3 P -0.577(5) 0.7168(11) 0.207(5) 0.33(3) Uani 0.270(11) 1 d . U P . .
C1 C -1.415(2) 0.6853(5) 0.8323(11) 0.058(4) Uani 1 1 d . . . . .
H1 H -1.4786 0.6928 0.8941 0.069 Uiso 1 1 calc R U . . .
C2 C -1.240(2) 0.6602(5) 0.8373(12) 0.059(4) Uani 1 1 d . . . . .
H2 H -1.1824 0.6527 0.9014 0.070 Uiso 1 1 calc R U . . .
C3 C -1.1529(13) 0.6465(3) 0.7463(12) 0.043(2) Uani 1 1 d . . . . .
C4 C -1.244(2) 0.6599(4) 0.6519(11) 0.055(4) Uani 1 1 d . . . . .
H4 H -1.1923 0.6500 0.5888 0.066 Uiso 1 1 calc R U . . .
C5 C -1.408(2) 0.6876(4) 0.6527(11) 0.054(4) Uani 1 1 d . . . . .
H5 H -1.4593 0.6985 0.5899 0.065 Uiso 1 1 calc R U . . .
C6 C -0.9633(14) 0.6211(3) 0.7440(11) 0.046(3) Uani 1 1 d . . . . .
C7 C -0.322(2) 0.5517(5) 1.0325(11) 0.064(4) Uani 1 1 d . . . . .
H7 H -0.2078 0.5339 1.0342 0.077 Uiso 1 1 calc R U . . .
C8 C -0.421(2) 0.5567(5) 0.9390(9) 0.062(4) Uani 1 1 d . . . . .
H8 H -0.3682 0.5439 0.8792 0.074 Uiso 1 1 calc R U . . .
C9 C -0.596(2) 0.5803(5) 0.9331(9) 0.046(3) Uani 1 1 d . . . . .
C10 C -0.664(3) 0.5969(8) 1.0222(11) 0.131(10) Uani 1 1 d . . . . .
H10 H -0.7862 0.6120 1.0235 0.158 Uiso 1 1 calc R U . . .
C11 C -0.552(3) 0.5917(9) 1.1130(12) 0.138(10) Uani 1 1 d . . . . .
H11 H -0.6033 0.6041 1.1736 0.165 Uiso 1 1 calc R U . . .
C12 C -0.703(2) 0.5895(4) 0.8340(9) 0.044(3) Uani 1 1 d . . . . .
C13 C -0.527(3) 0.6038(6) 0.3845(11) 0.099(7) Uani 1 1 d . . . . .
H13 H -0.5518 0.6225 0.3283 0.119 Uiso 1 1 calc R U . . .
C14 C -0.648(2) 0.6073(7) 0.4709(11) 0.097(7) Uani 1 1 d . . . . .
H14 H -0.7627 0.6250 0.4693 0.117 Uiso 1 1 calc R U . . .
C15 C -0.5963(19) 0.5843(4) 0.5592(9) 0.043(3) Uani 1 1 d . . . . .
C16 C -0.436(2) 0.5549(5) 0.5541(10) 0.058(4) Uani 1 1 d . . . . .
H16 H -0.3987 0.5380 0.6118 0.069 Uiso 1 1 calc R U . . .
C17 C -0.331(2) 0.5514(4) 0.4616(10) 0.060(4) Uani 1 1 d . . . . .
H17 H -0.2246 0.5314 0.4583 0.072 Uiso 1 1 calc R U . . .
C18 C -0.703(2) 0.5914(5) 0.6583(10) 0.048(3) Uani 1 1 d . . . . .
N1 N -1.4965(12) 0.6993(3) 0.7411(11) 0.059(3) Uani 1 1 d . . . . .
N2 N -0.3789(18) 0.5706(5) 1.1204(8) 0.066(4) Uani 1 1 d . . . . .
N3 N -0.3750(18) 0.5749(4) 0.3775(8) 0.056(3) Uani 1 1 d . . . . .
N4 N -0.8797(17) 0.6106(3) 0.8380(7) 0.047(3) Uani 1 1 d . . . . .
N5 N -0.6066(11) 0.5786(3) 0.7455(9) 0.045(2) Uani 1 1 d . . . . .
N6 N -0.8791(16) 0.6130(4) 0.6547(8) 0.048(3) Uani 1 1 d . . . . .
Zn1 Zn -1.7159(3) 0.7500 0.7413(3) 0.0682(6) Uani 1 2 d S T P . .
Zn2 Zn -0.19135(17) 0.57565(4) 0.24938(14) 0.0544(3) Uani 1 1 d . . . . .
I1 I -1.8823(3) 0.7500 0.91777(16) 0.0942(6) Uani 1 2 d S T P . .
I2 I -1.8831(3) 0.7500 0.56217(16) 0.0927(6) Uani 1 2 d S T P . .
I3 I -0.03758(16) 0.65186(3) 0.23963(15) 0.1181(5) Uani 1 1 d . . . . .
I4 I 0.04167(13) 0.50820(3) 0.25580(10) 0.0752(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
P1 P3 2.04(7) 4_575 ?
P1 P3 2.04(7) . ?
P1 P2 2.09(9) . ?
P2 P3 2.10(8) 4_575 ?
P2 P3 2.10(8) . ?
P3 P3 2.01(7) 4_575 ?
C1 N1 1.351(16) . ?
C1 C2 1.381(19) . ?
C2 C3 1.369(18) . ?
C3 C4 1.407(17) . ?
C3 C6 1.468(13) . ?
C4 C5 1.371(18) . ?
C5 N1 1.326(16) . ?
C6 N6 1.300(15) . ?
C6 N4 1.359(15) . ?
C7 N2 1.319(16) . ?
C7 C8 1.368(17) . ?
C8 C9 1.358(19) . ?
C9 C10 1.327(18) . ?
C9 C12 1.476(16) . ?
C10 C11 1.38(2) . ?
C11 N2 1.31(2) . ?
C12 N4 1.330(16) . ?
C12 N5 1.347(14) . ?
C13 N3 1.331(19) . ?
C13 C14 1.37(2) . ?
C14 C15 1.369(18) . ?
C15 C16 1.384(18) . ?
C15 C18 1.474(17) . ?
C16 C17 1.381(17) . ?
C17 N3 1.321(16) . ?
C18 N6 1.332(16) . ?
C18 N5 1.339(15) . ?
N1 Zn1 2.108(9) . ?
N2 Zn2 2.063(11) 1_556 ?
N3 Zn2 2.050(11) . ?
Zn1 N1 2.108(9) 4_575 ?
Zn1 I1 2.524(4) . ?
Zn1 I2 2.539(4) . ?
Zn2 N2 2.063(11) 1_554 ?
Zn2 I3 2.5190(17) . ?
Zn2 I4 2.5536(14) . ?

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
P3 P1 P3 59(3) 4_575 . ?
P3 P1 P2 61(3) 4_575 . ?
P3 P1 P2 61(3) . . ?
P1 P2 P3 58(3) . 4_575 ?
P1 P2 P3 58(3) . . ?
P3 P2 P3 57(3) 4_575 . ?
P3 P3 P1 60.6(15) 4_575 . ?
P3 P3 P2 61.5(15) 4_575 . ?
P1 P3 P2 61(2) . . ?
N1 C1 C2 122.7(13) . . ?
C3 C2 C1 118.9(13) . . ?
C2 C3 C4 117.8(9) . . ?
C2 C3 C6 122.7(13) . . ?
C4 C3 C6 119.4(13) . . ?
C5 C4 C3 120.1(12) . . ?
N1 C5 C4 121.5(13) . . ?
N6 C6 N4 124.3(9) . . ?
N6 C6 C3 119.2(13) . . ?
N4 C6 C3 116.3(12) . . ?
N2 C7 C8 124.4(14) . . ?
C9 C8 C7 120.3(13) . . ?
C10 C9 C8 116.2(13) . . ?
C10 C9 C12 120.5(13) . . ?
C8 C9 C12 123.2(11) . . ?
C9 C10 C11 120.0(16) . . ?
N2 C11 C10 125.2(15) . . ?
N4 C12 N5 124.8(10) . . ?
N4 C12 C9 118.1(11) . . ?
N5 C12 C9 116.9(12) . . ?
N3 C13 C14 123.2(14) . . ?
C15 C14 C13 119.0(15) . . ?
C14 C15 C16 118.1(12) . . ?
C14 C15 C18 121.4(13) . . ?
C16 C15 C18 120.5(12) . . ?
C17 C16 C15 118.6(12) . . ?
N3 C17 C16 123.5(13) . . ?
N6 C18 N5 125.3(11) . . ?
N6 C18 C15 117.8(12) . . ?
N5 C18 C15 116.7(12) . . ?
C5 N1 C1 118.7(9) . . ?
C5 N1 Zn1 120.1(9) . . ?
C1 N1 Zn1 119.8(10) . . ?
C11 N2 C7 113.6(13) . . ?
C11 N2 Zn2 122.6(11) . 1_556 ?
C7 N2 Zn2 123.0(10) . 1_556 ?
C17 N3 C13 117.2(12) . . ?
C17 N3 Zn2 122.2(9) . . ?
C13 N3 Zn2 119.8(10) . . ?
C12 N4 C6 115.3(9) . . ?
C18 N5 C12 114.0(8) . . ?
C6 N6 C18 116.2(11) . . ?
N1 Zn1 N1 93.2(5) . 4_575 ?
N1 Zn1 I1 107.8(4) . . ?
N1 Zn1 I1 107.8(4) 4_575 . ?
N1 Zn1 I2 107.0(4) . . ?
N1 Zn1 I2 107.0(4) 4_575 . ?
I1 Zn1 I2 128.42(8) . . ?
N3 Zn2 N2 106.6(3) . 1_554 ?
N3 Zn2 I3 106.9(3) . . ?
N2 Zn2 I3 105.5(4) 1_554 . ?
N3 Zn2 I4 109.0(3) . . ?
N2 Zn2 I4 108.9(4) 1_554 . ?
I3 Zn2 I4 119.17(6) . . ?

_refine_diff_density_max         1.661
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.110

