# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_4_sq
_database_code_depnum_ccdc_archive 'CCDC 1854604'
_audit_update_record             
;
2018-07-08 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_audit_creation_date             2018-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C96 H80 Mo48 N32 O144 Zn16), 4(O2 P0.5)'
_chemical_formula_sum            'C48 H40 Mo24 N16 O80 P2 Zn8'
_chemical_formula_weight         5008.42
_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 0.0033 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-x+1/2, y, -z+1/2'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-x+1, y+1/2, -z+1'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'x-1/2, -y, z-1/2'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'x, -y+1/2, z'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   27.560(4)
_cell_length_b                   27.560(4)
_cell_length_c                   12.012(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9124(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    33264
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      3.16
_shelx_estimated_absorpt_T_max   0.948
_shelx_estimated_absorpt_T_min   0.923
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4716
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1198
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32676
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        24.991
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         3.159
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_target            ?
_diffrn_source_type              ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1720
_reflns_number_total             2068
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.217
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2068
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0669
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0870P)²+155.9737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1782
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1 times of:
  H4 of C4, H3 of C3
 At 1.2 times of:
  H1 of C1, H7 of C7, H5 of C5
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim N1 \\sim N2: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C7(H7)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Mo1 Mo 0.05398(5) 0.250000 0.16708(9) 0.0461(4) Uani 1 2 d S T P . .
Mo2 Mo 0.11349(3) 0.18819(3) -0.04264(7) 0.0517(3) Uani 1 1 d . . . . .
Zn1 Zn 0.000000 0.14697(6) 0.05240(13) 0.0540(5) Uani 1 2 d S T P . .
P1 P 0.000000 0.250000 -0.125000 0.0272(11) Uani 1 8 d S T P . .
O1 O 0.0667(4) 0.250000 0.3028(8) 0.061(3) Uani 1 2 d S T P . .
O2 O 0.0955(2) 0.2004(2) 0.1126(5) 0.0471(15) Uani 1 1 d . . . . .
O3 O 0.0574(3) 0.1452(2) -0.0457(6) 0.0526(16) Uani 1 1 d . . . . .
O4 O 0.0454(3) 0.250000 -0.0499(7) 0.0389(18) Uani 1 2 d S T P . .
O5 O 0.000000 0.2960(3) 0.1492(7) 0.0396(19) Uani 1 2 d S T P . .
O6 O 0.1608(3) 0.1514(3) -0.0257(7) 0.074(2) Uani 1 1 d . . . . .
O9 O 0.1453(3) 0.250000 -0.0478(7) 0.044(2) Uani 1 2 d S T P . .
N1 N 0.000000 0.0885(6) 0.1457(13) 0.089(3) Uani 1 2 d S TU P . .
N2 N 0.000000 0.0385(6) 0.2830(14) 0.090(3) Uani 1 2 d S TU P . .
C1 C 0.000000 0.0817(7) 0.2506(17) 0.088(3) Uani 1 2 d S TU P . .
H1 H 0.000000 0.107451 0.300613 0.105 Uiso 1 2 calc RS T P . .
C2 C 0.000000 0.0187(8) 0.3959(16) 0.087(3) Uani 1 2 d S TU P . .
C3 C 0.000000 -0.0290(8) 0.4056(17) 0.091(3) Uani 1 2 d S TU P . .
H3 H 0.000000 -0.048906 0.343097 0.091 Uiso 1 2 calc RS T P . .
C4 C 0.000000 0.0486(8) 0.4859(17) 0.090(3) Uani 1 2 d S TU P . .
H4 H 0.000000 0.082108 0.475889 0.090 Uiso 1 2 calc RS T P . .
C5 C 0.000000 0.0117(8) 0.1896(17) 0.095(3) Uani 1 2 d S TU P . .
H5 H 0.000000 -0.022029 0.185521 0.114 Uiso 1 2 calc RS T P . .
C7 C 0.000000 0.0437(8) 0.1004(18) 0.095(3) Uani 1 2 d S TU P . .
H7 H 0.000000 0.035862 0.025069 0.114 Uiso 1 2 calc RS T P . .


_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
Mo1 Mo1 2.975(3) 11_454 ?
Mo1 O1 1.667(10) . ?
Mo1 O2 1.899(6) 31 ?
Mo1 O2 1.899(6) . ?
Mo1 O5 1.967(6) . ?
Mo1 O5 1.967(6) 11_454 ?
Mo2 Mo2 2.8234(19) 8_554 ?
Mo2 O2 1.959(6) . ?
Mo2 O3 1.948(7) . ?
Mo2 O3 1.960(7) 8_554 ?
Mo2 O6 1.664(7) . ?
Mo2 O9 1.917(4) . ?
Zn1 O3 1.974(7) . ?
Zn1 O3 1.974(7) 21 ?
Zn1 O5 1.955(9) 11_454 ?
Zn1 N1 1.962(16) . ?
P1 O4 1.543(8) 28 ?
P1 O4 1.543(8) . ?
P1 O4 1.543(8) 11_454 ?
P1 O4 1.543(8) 18_565 ?
N1 C1 1.28(2) . ?
N1 C7 1.35(3) . ?
N2 C1 1.25(2) . ?
N2 C2 1.46(2) . ?
N2 C5 1.34(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.32(3) . ?
C2 C4 1.36(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.41(3) 17_556 ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C5 C7 1.39(3) . ?
C7 H7 0.9300 . ?

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
O1 Mo1 Mo1 102.2(4) . 11_454 ?
O1 Mo1 O2 102.1(3) . . ?
O1 Mo1 O2 102.1(3) . 31 ?
O1 Mo1 O5 105.4(4) . . ?
O1 Mo1 O5 105.4(4) . 11_454 ?
O2 Mo1 Mo1 127.0(2) 31 11_454 ?
O2 Mo1 Mo1 127.0(2) . 11_454 ?
O2 Mo1 O2 92.1(4) . 31 ?
O2 Mo1 O5 151.9(3) . . ?
O2 Mo1 O5 87.3(3) 31 . ?
O2 Mo1 O5 151.9(3) 31 11_454 ?
O2 Mo1 O5 87.3(3) . 11_454 ?
O5 Mo1 Mo1 40.85(19) . 11_454 ?
O5 Mo1 Mo1 40.86(19) 11_454 11_454 ?
O5 Mo1 O5 80.3(4) . 11_454 ?
O2 Mo2 Mo2 128.7(2) . 8_554 ?
O2 Mo2 O3 154.4(3) . 8_554 ?
O3 Mo2 Mo2 43.9(2) . 8_554 ?
O3 Mo2 Mo2 43.6(2) 8_554 8_554 ?
O3 Mo2 O2 85.5(3) . . ?
O3 Mo2 O3 85.5(3) . 8_554 ?
O6 Mo2 Mo2 100.0(3) . 8_554 ?
O6 Mo2 O2 100.8(3) . . ?
O6 Mo2 O3 104.7(3) . 8_554 ?
O6 Mo2 O3 104.7(4) . . ?
O6 Mo2 O9 100.7(4) . . ?
O9 Mo2 Mo2 131.0(2) . 8_554 ?
O9 Mo2 O2 89.7(3) . . ?
O9 Mo2 O3 154.6(3) . . ?
O9 Mo2 O3 88.2(3) . 8_554 ?
O3 Zn1 O3 106.6(4) . 21 ?
O5 Zn1 O3 112.0(2) 11_454 21 ?
O5 Zn1 O3 112.0(2) 11_454 . ?
O5 Zn1 N1 108.7(6) 11_454 . ?
N1 Zn1 O3 108.7(3) . 21 ?
N1 Zn1 O3 108.7(3) . . ?
O4 P1 O4 110.0(3) 28 11_454 ?
O4 P1 O4 110.0(3) . 18_565 ?
O4 P1 O4 108.4(6) 18_565 28 ?
O4 P1 O4 110.0(3) 18_565 11_454 ?
O4 P1 O4 110.0(3) . 28 ?
O4 P1 O4 108.4(6) . 11_454 ?
Mo1 O2 Mo2 127.2(3) . . ?
Mo2 O3 Mo2 92.5(3) . 8_554 ?
Mo2 O3 Zn1 127.6(4) . . ?
Mo2 O3 Zn1 130.1(4) 8_554 . ?
Mo1 O5 Mo1 98.3(4) . 11_454 ?
Zn1 O5 Mo1 125.7(2) 11_454 11_454 ?
Zn1 O5 Mo1 125.7(2) 11_454 . ?
Mo2 O9 Mo2 125.4(4) . 31 ?
C1 N1 Zn1 133.3(15) . . ?
C1 N1 C7 105.2(17) . . ?
C7 N1 Zn1 121.4(13) . . ?
C1 N2 C2 130.1(19) . . ?
C1 N2 C5 105.3(18) . . ?
C5 N2 C2 124.6(18) . . ?
N1 C1 H1 121.7 . . ?
N2 C1 N1 117(2) . . ?
N2 C1 H1 121.7 . . ?
C3 C2 N2 117.0(19) . . ?
C3 C2 C4 122.4(19) . . ?
C4 C2 N2 120.6(19) . . ?
C2 C3 H3 121.2 . . ?
C2 C3 C4 118(2) . 17_556 ?
C4 C3 H3 121.2 17_556 . ?
C2 C4 C3 120(2) . 17_556 ?
C2 C4 H4 120.0 . . ?
C3 C4 H4 120.0 17_556 . ?
N2 C5 H5 126.4 . . ?
N2 C5 C7 107(2) . . ?
C7 C5 H5 126.4 . . ?
N1 C7 C5 105.7(19) . . ?
N1 C7 H7 127.1 . . ?
C5 C7 H7 127.1 . . ?

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
Mo1 Mo1 O2 Mo2 80.0(5) 11_454 . . . ?
Zn1 N1 C1 N2 180.000(1) . . . . ?
Zn1 N1 C7 C5 180.000(1) . . . . ?
O1 Mo1 O2 Mo2 -164.4(5) . . . . ?
O2 Mo1 O2 Mo2 -61.5(5) 31 . . . ?
O5 Mo1 O2 Mo2 90.4(5) 11_454 . . . ?
O5 Mo1 O2 Mo2 26.8(9) . . . . ?
N2 C2 C3 C4 180.000(2) . . . 17_556 ?
N2 C2 C4 C3 180.000(3) . . . 17_556 ?
N2 C5 C7 N1 0.000(2) . . . . ?
C1 N1 C7 C5 0.000(2) . . . . ?
C1 N2 C2 C3 180.000(2) . . . . ?
C1 N2 C2 C4 0.000(3) . . . . ?
C1 N2 C5 C7 0.000(1) . . . . ?
C2 N2 C1 N1 180.000(2) . . . . ?
C2 N2 C5 C7 180.000(2) . . . . ?
C3 C2 C4 C3 0.000(4) . . . 17_556 ?
C4 C2 C3 C4 0.000(3) . . . 17_556 ?
C5 N2 C1 N1 0.000(2) . . . . ?
C5 N2 C2 C3 0.000(3) . . . . ?
C5 N2 C2 C4 180.000(3) . . . . ?
C7 N1 C1 N2 0.000(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
