# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_L1-Zr-Ir
_database_code_depnum_ccdc_archive 'CCDC 1436270'
_audit_update_record             
;
2015-11-11 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Ir-POF-1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C144 H72 Cl3 Ir3 N12 O64 Zr12'
_chemical_formula_weight         4771.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'

_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, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   38.3937(2)
_cell_length_b                   38.3937(2)
_cell_length_c                   38.3937(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     56595.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5091
_cell_measurement_theta_min      3.6410
_cell_measurement_theta_max      64.6490

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.560
_exptl_crystal_F_000             9176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.421
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.726
_exptl_absorpt_correction_T_min  0.64151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measurement_method       ?
_diffrn_reflns_number            18180
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.640
_diffrn_reflns_theta_max         64.657
_diffrn_reflns_theta_full        64.657
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4393
_reflns_number_gt                3298
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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.

The molecules in the crystal show apparent disorder but not 
treated due to too high symmetry, which causing significant
ADP max/min ratio especially for Ir and Zr atoms.
All solvent molecules are removed by SQUEEZE program. 
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1790P)²+38.0617P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0000081(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4393
_refine_ls_number_parameters     103
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.2559
_refine_ls_wR_factor_gt          0.2396
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.346
_refine_ls_shift/su_max          0.008
_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
Ir1 Ir 0.5000 1.0000 0.2500 0.1671(5) Uani 1 8 d S TU P . .
Zr1 Zr 0.70694(2) 0.77136(2) 0.29306(2) 0.14892(17) Uani 1 2 d S TU P . .
N1 N 0.5000 0.94695(14) 0.2497(3) 0.136(3) Uani 1 2 d S TU P . .
O1 O 0.67214(11) 0.81407(10) 0.27850(12) 0.1462(14) Uani 1 1 d . U . . .
O2 O 0.74272(12) 0.8078(2) 0.25728(12) 0.194(3) Uani 1 2 d S TU P . .
O3 O 0.71713(15) 0.71713(15) 0.28287(15) 0.0884(18) Uani 1 6 d S TU P . .
O4 O 0.65259(14) 0.74958(15) 0.29986(19) 0.196(2) Uani 1 1 d . U . . .
Cl1 Cl 0.5000 1.0000 0.1899(5) 0.272(5) Uani 0.5 4 d S TU P . .
C1 C 0.66931(13) 0.83069(13) 0.2500 0.131(3) Uani 1 2 d DS TU P . .
C2 C 0.64101(11) 0.85899(11) 0.2500 0.122(3) Uani 1 2 d DS TU P . .
C3 C 0.63332(16) 0.87617(17) 0.2202(2) 0.150(2) Uani 1 1 d D U . . .
H3 H 0.6450 0.8703 0.1992 0.180 Uiso 1 1 calc R U . . .
C4 C 0.60839(16) 0.90240(17) 0.22040(17) 0.151(2) Uani 1 1 d D U . . .
H4 H 0.6039 0.9153 0.1998 0.182 Uiso 1 1 calc R U . . .
C5 C 0.59039(11) 0.90961(11) 0.2500 0.131(3) Uani 1 2 d DS TU P . .
C6 C 0.56278(10) 0.93722(10) 0.2500 0.132(3) Uani 1 2 d DS TU P . .
C7 C 0.52882(12) 0.92662(12) 0.2485(2) 0.141(2) Uani 1 1 d . U . . .
C8 C 0.51743(13) 0.89068(13) 0.2478(2) 0.156(3) Uani 1 1 d . U . . .
H8 H 0.5321 0.8707 0.2475 0.188 Uiso 1 1 calc R U . . .


_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
Ir1 N1 2.037(5) . ?
Ir1 N1 2.037(5) 38_665 ?
Ir1 N1 2.037(5) 37_455 ?
Ir1 N1 2.037(5) 2_675 ?
Ir1 Cl1 2.308(19) 37_455 ?
Ir1 Cl1 2.308(19) . ?
Zr1 O2 2.085(3) 83_654 ?
Zr1 O2 2.085(3) 80_564 ?
Zr1 O3 2.154(4) . ?
Zr1 O1 2.188(4) . ?
Zr1 O1 2.188(4) 70_656 ?
Zr1 O4 2.263(6) 70_656 ?
Zr1 O4 2.263(6) . ?
Zr1 O2 2.394(9) . ?
Zr1 Zr1 3.4972(9) 8_656 ?
Zr1 Zr1 3.4972(9) 11_566 ?
Zr1 Zr1 3.5097(15) 80_564 ?
Zr1 Zr1 3.5097(14) 83_654 ?
N1 C7 1.355(5) 52_655 ?
N1 C7 1.355(5) . ?
O1 C1 1.271(5) . ?
O2 Zr1 2.085(3) 83_654 ?
O2 Zr1 2.085(3) 80_564 ?
O3 Zr1 2.154(3) 8_656 ?
O3 Zr1 2.154(4) 11_566 ?
C1 O1 1.271(5) 38_665 ?
C1 C2 1.537(9) . ?
C2 C3 1.352(7) . ?
C2 C3 1.352(7) 38_665 ?
C3 C4 1.389(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.359(6) . ?
C4 H4 0.9500 . ?
C5 C4 1.359(6) 38_665 ?
C5 C6 1.499(8) . ?
C6 C7 1.367(5) . ?
C6 C7 1.367(5) 38_665 ?
C7 C8 1.447(7) . ?
C8 C8 1.339(10) 52_655 ?
C8 H8 0.9500 . ?

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
N1 Ir1 N1 90.002(5) . 38_665 ?
N1 Ir1 N1 90.002(6) . 37_455 ?
N1 Ir1 N1 179.4(6) 38_665 37_455 ?
N1 Ir1 N1 179.4(6) . 2_675 ?
N1 Ir1 N1 90.002(5) 38_665 2_675 ?
N1 Ir1 N1 90.002(5) 37_455 2_675 ?
N1 Ir1 Cl1 90.3(3) . 37_455 ?
N1 Ir1 Cl1 89.7(3) 38_665 37_455 ?
N1 Ir1 Cl1 89.7(3) 37_455 37_455 ?
N1 Ir1 Cl1 90.3(3) 2_675 37_455 ?
N1 Ir1 Cl1 89.7(3) . . ?
N1 Ir1 Cl1 90.3(3) 38_665 . ?
N1 Ir1 Cl1 90.3(3) 37_455 . ?
N1 Ir1 Cl1 89.7(3) 2_675 . ?
Cl1 Ir1 Cl1 180.0 37_455 . ?
O2 Zr1 O2 115.9(4) 83_654 80_564 ?
O2 Zr1 O3 68.32(18) 83_654 . ?
O2 Zr1 O3 68.32(18) 80_564 . ?
O2 Zr1 O1 77.97(19) 83_654 . ?
O2 Zr1 O1 146.1(2) 80_564 . ?
O3 Zr1 O1 142.09(11) . . ?
O2 Zr1 O1 146.1(2) 83_654 70_656 ?
O2 Zr1 O1 77.97(19) 80_564 70_656 ?
O3 Zr1 O1 142.09(11) . 70_656 ?
O1 Zr1 O1 75.5(2) . 70_656 ?
O2 Zr1 O4 136.7(3) 83_654 70_656 ?
O2 Zr1 O4 76.1(3) 80_564 70_656 ?
O3 Zr1 O4 80.3(2) . 70_656 ?
O1 Zr1 O4 116.2(2) . 70_656 ?
O1 Zr1 O4 75.12(19) 70_656 70_656 ?
O2 Zr1 O4 76.1(3) 83_654 . ?
O2 Zr1 O4 136.7(3) 80_564 . ?
O3 Zr1 O4 80.3(2) . . ?
O1 Zr1 O4 75.12(19) . . ?
O1 Zr1 O4 116.2(2) 70_656 . ?
O4 Zr1 O4 69.6(4) 70_656 . ?
O2 Zr1 O2 77.0(3) 83_654 . ?
O2 Zr1 O2 77.0(3) 80_564 . ?
O3 Zr1 O2 110.9(3) . . ?
O1 Zr1 O2 76.44(18) . . ?
O1 Zr1 O2 76.44(18) 70_656 . ?
O4 Zr1 O2 144.20(17) 70_656 . ?
O4 Zr1 O2 144.21(17) . . ?
O2 Zr1 Zr1 33.01(14) 83_654 8_656 ?
O2 Zr1 Zr1 90.51(17) 80_564 8_656 ?
O3 Zr1 Zr1 35.73(13) . 8_656 ?
O1 Zr1 Zr1 110.45(11) . 8_656 ?
O1 Zr1 Zr1 164.12(12) 70_656 8_656 ?
O4 Zr1 Zr1 113.01(14) 70_656 8_656 ?
O4 Zr1 Zr1 79.66(16) . 8_656 ?
O2 Zr1 Zr1 90.45(15) . 8_656 ?
O2 Zr1 Zr1 90.51(17) 83_654 11_566 ?
O2 Zr1 Zr1 33.01(14) 80_564 11_566 ?
O3 Zr1 Zr1 35.73(13) . 11_566 ?
O1 Zr1 Zr1 164.12(12) . 11_566 ?
O1 Zr1 Zr1 110.45(11) 70_656 11_566 ?
O4 Zr1 Zr1 79.66(16) 70_656 11_566 ?
O4 Zr1 Zr1 113.01(14) . 11_566 ?
O2 Zr1 Zr1 90.45(15) . 11_566 ?
Zr1 Zr1 Zr1 60.0 8_656 11_566 ?
O2 Zr1 Zr1 95.6(3) 83_654 80_564 ?
O2 Zr1 Zr1 41.7(2) 80_564 80_564 ?
O3 Zr1 Zr1 90.9(2) . 80_564 ?
O1 Zr1 Zr1 109.68(12) . 80_564 ?
O1 Zr1 Zr1 74.13(12) 70_656 80_564 ?
O4 Zr1 Zr1 114.54(18) 70_656 80_564 ?
O4 Zr1 Zr1 169.62(16) . 80_564 ?
O2 Zr1 Zr1 35.38(9) . 80_564 ?
Zr1 Zr1 Zr1 90.0 8_656 80_564 ?
Zr1 Zr1 Zr1 60.114(13) 11_566 80_564 ?
O2 Zr1 Zr1 41.7(2) 83_654 83_654 ?
O2 Zr1 Zr1 95.6(3) 80_564 83_654 ?
O3 Zr1 Zr1 90.9(2) . 83_654 ?
O1 Zr1 Zr1 74.13(12) . 83_654 ?
O1 Zr1 Zr1 109.68(12) 70_656 83_654 ?
O4 Zr1 Zr1 169.62(16) 70_656 83_654 ?
O4 Zr1 Zr1 114.54(18) . 83_654 ?
O2 Zr1 Zr1 35.38(9) . 83_654 ?
Zr1 Zr1 Zr1 60.114(13) 8_656 83_654 ?
Zr1 Zr1 Zr1 90.0 11_566 83_654 ?
Zr1 Zr1 Zr1 59.76(3) 80_564 83_654 ?
C7 N1 C7 109.5(6) 52_655 . ?
C7 N1 Ir1 125.2(3) 52_655 . ?
C7 N1 Ir1 125.2(3) . . ?
C1 O1 Zr1 130.4(4) . . ?
Zr1 O2 Zr1 114.0(3) 83_654 80_564 ?
Zr1 O2 Zr1 102.9(3) 83_654 . ?
Zr1 O2 Zr1 102.9(3) 80_564 . ?
Zr1 O3 Zr1 108.5(3) 8_656 11_566 ?
Zr1 O3 Zr1 108.5(3) 8_656 . ?
Zr1 O3 Zr1 108.5(3) 11_566 . ?
O1 C1 O1 130.9(7) 38_665 . ?
O1 C1 C2 114.5(3) 38_665 . ?
O1 C1 C2 114.5(3) . . ?
C3 C2 C3 120.1(7) . 38_665 ?
C3 C2 C1 120.0(4) . . ?
C3 C2 C1 120.0(4) 38_665 . ?
C2 C3 C4 120.0(7) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.1(7) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C4 119.5(7) 38_665 . ?
C4 C5 C6 120.2(4) 38_665 . ?
C4 C5 C6 120.2(4) . . ?
C7 C6 C7 124.7(6) . 38_665 ?
C7 C6 C5 117.6(3) . . ?
C7 C6 C5 117.6(3) 38_665 . ?
N1 C7 C6 127.3(5) . . ?
N1 C7 C8 107.7(4) . . ?
C6 C7 C8 124.9(4) . . ?
C8 C8 C7 107.6(3) 52_655 . ?
C8 C8 H8 126.2 52_655 . ?
C7 C8 H8 126.2 . . ?

_refine_diff_density_max         1.276
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.094



