# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1587925'
_audit_update_record             
;
2017-12-27 deposited with the CCDC.
2017-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H18 N O16 P4 Zn3'
_chemical_formula_weight         716.23

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.1301(10)
_cell_length_b                   11.6623(14)
_cell_length_c                   11.8071(17)
_cell_angle_alpha                78.467(11)
_cell_angle_beta                 78.512(11)
_cell_angle_gamma                84.936(10)
_cell_volume                     1073.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2091
_cell_measurement_theta_min      3.2100
_cell_measurement_theta_max      31.4500

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_F_000             714
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    3.703
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5508
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.755
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_full        25.010
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3784
_reflns_number_gt                3247
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_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+5.6000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3784
_refine_ls_number_parameters     300
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_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
C1 C 0.2011(6) 0.6911(5) 0.9380(4) 0.0232(11) Uani 1 1 d . . . . .
C2 C 0.2678(9) 0.6113(5) 1.0371(5) 0.0400(16) Uani 1 1 d . . . . .
H2A H 0.187717 0.610443 1.108926 0.060 Uiso 1 1 calc R U . . .
H2B H 0.371846 0.639037 1.045184 0.060 Uiso 1 1 calc R U . . .
H2C H 0.286601 0.533439 1.020436 0.060 Uiso 1 1 calc R U . . .
C3 C 0.5956(6) 1.1320(4) 0.7206(4) 0.0171(10) Uani 1 1 d . . . . .
C4 C 0.6289(7) 1.2593(5) 0.7099(5) 0.0273(12) Uani 1 1 d . . . . .
H4A H 0.530698 1.298871 0.747284 0.041 Uiso 1 1 calc R U . . .
H4B H 0.655667 1.294930 0.628281 0.041 Uiso 1 1 calc R U . . .
H4C H 0.721622 1.265017 0.747373 0.041 Uiso 1 1 calc R U . . .
C5 C 0.9037(7) 0.7510(5) 0.5339(5) 0.0312(13) Uani 1 1 d . . . . .
H5 H 0.901471 0.828364 0.494209 0.037 Uiso 1 1 calc R U . . .
C6 C 0.9592(7) 0.6623(5) 0.4729(5) 0.0332(13) Uani 1 1 d . . . . .
H6 H 0.990134 0.679376 0.391427 0.040 Uiso 1 1 calc R U . . .
C7 C 0.9694(7) 0.5486(5) 0.5313(5) 0.0293(12) Uani 1 1 d . . . . .
C8 C 0.9140(13) 0.5291(6) 0.6528(6) 0.083(3) Uani 1 1 d . . . . .
H8 H 0.918826 0.453375 0.696148 0.099 Uiso 1 1 calc R U . . .
C9 C 0.8539(15) 0.6180(7) 0.7080(6) 0.093(4) Uani 1 1 d . . . . .
H9 H 0.812040 0.603592 0.788514 0.111 Uiso 1 1 calc R U . . .
N1 N 0.8542(7) 0.7269(4) 0.6472(4) 0.0436(14) Uani 1 1 d . . . . .
H1 H 0.820398 0.783613 0.684276 0.052 Uiso 1 1 calc R U . . .
O1 O 0.3294(4) 0.8884(3) 0.9701(3) 0.0227(8) Uani 1 1 d . . . . .
O2 O 0.0666(5) 0.9109(3) 0.8804(3) 0.0272(8) Uani 1 1 d . . . . .
O3 O 0.0536(5) 0.8213(3) 1.0934(3) 0.0270(8) Uani 1 1 d . . . . .
O4 O 0.2710(5) 0.7396(3) 0.6965(3) 0.0303(9) Uani 1 1 d . . . . .
O5 O 0.5111(4) 0.7351(3) 0.8078(3) 0.0285(8) Uani 1 1 d . . . . .
O6 O 0.3946(5) 0.5499(3) 0.7993(3) 0.0359(10) Uani 1 1 d . . . . .
H6A H 0.332660 0.492283 0.805660 0.054 Uiso 1 1 d R U . . .
O7 O 0.7478(4) 0.9221(3) 0.7225(3) 0.0249(8) Uani 1 1 d . . . . .
O8 O 0.7910(4) 1.0615(4) 0.5255(3) 0.0281(9) Uani 1 1 d . . . . .
O9 O 0.9338(4) 1.0923(3) 0.6826(3) 0.0221(8) Uani 1 1 d . . . . .
O10 O 0.2602(4) 1.1663(3) 0.7304(3) 0.0222(8) Uani 1 1 d . . . . .
O11 O 0.4449(4) 1.1674(3) 0.5306(3) 0.0262(8) Uani 1 1 d . . . . .
O12 O 0.4020(4) 0.9776(3) 0.6821(3) 0.0244(8) Uani 1 1 d . . . . .
O13 O 0.0436(5) 0.6482(4) 0.9295(4) 0.0489(12) Uani 1 1 d . . . . .
H13A H 0.025816 0.670222 0.862425 0.059 Uiso 1 1 d R U . . .
O14 O 0.5493(4) 1.0767(3) 0.8445(3) 0.0194(7) Uani 1 1 d D . . . .
H14A H 0.595041 1.089728 0.908675 0.023 Uiso 1 1 d DR U . . .
O15 O 0.6999(5) 0.8440(4) 0.9690(3) 0.0379(10) Uani 1 1 d D . . . .
H15A H 0.817578 0.831567 0.957827 0.045 Uiso 1 1 d DR U . . .
H15B H 0.679178 0.846127 1.050672 0.045 Uiso 1 1 d DR U . . .
P1 P 0.16164(15) 0.83925(11) 0.97141(10) 0.0169(3) Uani 1 1 d . . . . .
P2 P 0.35139(17) 0.68350(12) 0.80061(11) 0.0224(3) Uani 1 1 d . . . . .
P3 P 0.78159(15) 1.04635(11) 0.65647(10) 0.0172(3) Uani 1 1 d . . . . .
P4 P 0.41333(15) 1.11155(11) 0.65945(10) 0.0167(3) Uani 1 1 d . . . . .
Zn1 Zn 0.53831(7) 0.88921(5) 0.84580(5) 0.02289(16) Uani 1 1 d D . . . .
Zn2 Zn 0.35632(7) 0.87430(5) 0.58279(5) 0.02038(16) Uani 1 1 d . . . . .
Zn3 Zn 1.06306(7) 1.07417(5) 0.80465(5) 0.01773(15) Uani 1 1 d . . . . .
O16 O 0.1871(8) 0.3778(6) 0.8278(7) 0.102(2) 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
C1 O13 1.444(6) . ?
C1 C2 1.502(7) . ?
C1 P1 1.835(5) . ?
C1 P2 1.839(5) . ?
C3 O14 1.464(5) . ?
C3 C4 1.508(7) . ?
C3 P4 1.825(5) . ?
C3 P3 1.855(5) . ?
C5 N1 1.298(7) . ?
C5 C6 1.371(8) . ?
C6 C7 1.371(8) . ?
C7 C8 1.394(8) . ?
C7 C7 1.471(11) 2_766 ?
C8 C9 1.339(10) . ?
C9 N1 1.328(9) . ?
O1 P1 1.521(3) . ?
O1 Zn1 2.011(3) . ?
O2 P1 1.519(4) . ?
O2 Zn3 1.935(4) 1_455 ?
O3 P1 1.516(3) . ?
O3 Zn3 1.940(4) 2_677 ?
O4 P2 1.513(4) . ?
O4 Zn2 1.931(4) . ?
O5 P2 1.502(4) . ?
O5 Zn1 1.979(4) . ?
O6 P2 1.569(4) . ?
O7 P3 1.522(4) . ?
O7 Zn1 2.018(3) . ?
O8 P3 1.508(3) . ?
O8 Zn2 1.924(4) 2_676 ?
O9 P3 1.500(3) . ?
O9 Zn3 1.915(3) . ?
O10 P4 1.523(3) . ?
O10 Zn3 1.964(3) 1_455 ?
O11 P4 1.511(3) . ?
O11 Zn2 1.975(3) 2_676 ?
O12 P4 1.539(4) . ?
O12 Zn2 1.945(3) . ?
O12 Zn1 2.425(3) . ?
O14 Zn1 2.193(4) . ?
O15 Zn1 2.110(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 C1 C2 108.1(5) . . ?
O13 C1 P1 108.6(4) . . ?
C2 C1 P1 109.4(4) . . ?
O13 C1 P2 108.6(3) . . ?
C2 C1 P2 108.3(4) . . ?
P1 C1 P2 113.8(3) . . ?
O14 C3 C4 110.5(4) . . ?
O14 C3 P4 103.1(3) . . ?
C4 C3 P4 113.0(4) . . ?
O14 C3 P3 106.7(3) . . ?
C4 C3 P3 112.7(3) . . ?
P4 C3 P3 110.2(2) . . ?
N1 C5 C6 119.9(5) . . ?
C7 C6 C5 120.4(5) . . ?
C6 C7 C8 116.5(5) . . ?
C6 C7 C7 121.8(6) . 2_766 ?
C8 C7 C7 121.6(6) . 2_766 ?
C9 C8 C7 120.9(7) . . ?
N1 C9 C8 119.7(7) . . ?
C5 N1 C9 122.5(6) . . ?
P1 O1 Zn1 127.4(2) . . ?
P1 O2 Zn3 133.6(2) . 1_455 ?
P1 O3 Zn3 134.3(2) . 2_677 ?
P2 O4 Zn2 123.6(2) . . ?
P2 O5 Zn1 127.9(2) . . ?
P3 O7 Zn1 120.5(2) . . ?
P3 O8 Zn2 135.7(2) . 2_676 ?
P3 O9 Zn3 140.6(2) . . ?
P4 O10 Zn3 120.5(2) . 1_455 ?
P4 O11 Zn2 123.2(2) . 2_676 ?
P4 O12 Zn2 131.1(2) . . ?
P4 O12 Zn1 109.50(17) . . ?
Zn2 O12 Zn1 117.07(17) . . ?
C3 O14 Zn1 105.9(3) . . ?
O3 P1 O1 111.6(2) . . ?
O3 P1 O2 111.4(2) . . ?
O1 P1 O2 113.2(2) . . ?
O3 P1 C1 104.1(2) . . ?
O1 P1 C1 108.5(2) . . ?
O2 P1 C1 107.3(2) . . ?
O5 P2 O4 115.7(2) . . ?
O5 P2 O6 106.5(2) . . ?
O4 P2 O6 110.3(2) . . ?
O5 P2 C1 108.0(2) . . ?
O4 P2 C1 109.6(2) . . ?
O6 P2 C1 106.3(2) . . ?
O9 P3 O8 110.6(2) . . ?
O9 P3 O7 112.6(2) . . ?
O8 P3 O7 113.7(2) . . ?
O9 P3 C3 107.3(2) . . ?
O8 P3 C3 109.5(2) . . ?
O7 P3 C3 102.6(2) . . ?
O11 P4 O10 113.1(2) . . ?
O11 P4 O12 113.8(2) . . ?
O10 P4 O12 110.0(2) . . ?
O11 P4 C3 108.3(2) . . ?
O10 P4 C3 107.4(2) . . ?
O12 P4 C3 103.8(2) . . ?
O5 Zn1 O1 96.29(14) . . ?
O5 Zn1 O7 94.14(14) . . ?
O1 Zn1 O7 169.28(15) . . ?
O5 Zn1 O15 101.77(17) . . ?
O1 Zn1 O15 93.77(15) . . ?
O7 Zn1 O15 86.50(15) . . ?
O5 Zn1 O14 165.37(14) . . ?
O1 Zn1 O14 88.05(13) . . ?
O7 Zn1 O14 81.23(13) . . ?
O15 Zn1 O14 91.84(15) . . ?
O5 Zn1 O12 87.59(14) . . ?
O1 Zn1 O12 95.66(13) . . ?
O7 Zn1 O12 82.29(13) . . ?
O15 Zn1 O12 165.90(14) . . ?
O14 Zn1 O12 78.06(12) . . ?
O8 Zn2 O4 113.54(16) 2_676 . ?
O8 Zn2 O12 116.21(16) 2_676 . ?
O4 Zn2 O12 102.44(14) . . ?
O8 Zn2 O11 99.06(14) 2_676 2_676 ?
O4 Zn2 O11 112.22(17) . 2_676 ?
O12 Zn2 O11 113.91(15) . 2_676 ?
O9 Zn3 O2 108.14(15) . 1_655 ?
O9 Zn3 O3 103.89(16) . 2_677 ?
O2 Zn3 O3 113.72(15) 1_655 2_677 ?
O9 Zn3 O10 103.65(14) . 1_655 ?
O2 Zn3 O10 126.18(16) 1_655 1_655 ?
O3 Zn3 O10 98.87(15) 2_677 1_655 ?

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.135



####################################################################### 
# 
# 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_1_sq_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1587926'
_audit_update_record             
;
2017-12-27 deposited with the CCDC.
2017-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 N4 O14 P4 Zn4'
_chemical_formula_weight         977.83

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.4871(4)
_cell_length_b                   13.1962(9)
_cell_length_c                   26.4829(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.505(4)
_cell_angle_gamma                90
_cell_volume                     3664.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3951
_cell_measurement_theta_min      2.7760
_cell_measurement_theta_max      30.9720

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             1952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.827
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13695
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.602
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_full        25.006
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6452
_reflns_number_gt                4942
_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.
;

_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+12.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6452
_refine_ls_number_parameters     453
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_restrained_S_all      0.921
_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
C1 C 0.6178(3) 0.2822(3) 0.08018(14) 0.0306(9) Uani 1 1 d . . . . .
C2 C 0.7100(4) 0.3354(4) 0.04685(15) 0.0405(11) Uani 1 1 d . . . . .
H2A H 0.742234 0.288628 0.022291 0.061 Uiso 1 1 calc R U . . .
H2B H 0.779441 0.361266 0.066884 0.061 Uiso 1 1 calc R U . . .
H2C H 0.667762 0.390410 0.029921 0.061 Uiso 1 1 calc R U . . .
C3 C 1.1301(4) 0.2641(3) 0.18207(14) 0.0324(10) Uani 1 1 d . . . . .
C4 C 1.0389(4) 0.2128(4) 0.21668(16) 0.0483(13) Uani 1 1 d . . . . .
H4A H 1.079800 0.155399 0.232130 0.073 Uiso 1 1 calc R U . . .
H4B H 0.965586 0.190481 0.197773 0.073 Uiso 1 1 calc R U . . .
H4C H 1.012682 0.259442 0.242385 0.073 Uiso 1 1 calc R U . . .
C5 C 0.8107(4) 0.3883(3) 0.29439(15) 0.0352(10) Uani 1 1 d . . . . .
H5 H 0.896589 0.379528 0.287146 0.042 Uiso 1 1 calc R U . . .
C6 C 0.7739(4) 0.3896(3) 0.34414(14) 0.0348(10) Uani 1 1 d . . . . .
H6 H 0.834513 0.381098 0.369655 0.042 Uiso 1 1 calc R U . . .
C7 C 0.6473(4) 0.4034(3) 0.35627(14) 0.0285(9) Uani 1 1 d . . . . .
C8 C 0.5636(4) 0.4198(3) 0.31643(15) 0.0379(11) Uani 1 1 d . . . . .
H8 H 0.478214 0.433440 0.322785 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6059(4) 0.4162(4) 0.26773(15) 0.0376(11) Uani 1 1 d . . . . .
H9 H 0.547334 0.425907 0.241596 0.045 Uiso 1 1 calc R U . . .
C10 C 0.6436(4) 0.3849(3) 0.49781(15) 0.0337(10) Uani 1 1 d . . . . .
H10 H 0.701947 0.387826 0.524431 0.040 Uiso 1 1 calc R U . . .
C11 C 0.6865(4) 0.3990(3) 0.44958(15) 0.0352(10) Uani 1 1 d . . . . .
H11 H 0.772664 0.410886 0.443981 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6017(4) 0.3955(3) 0.40904(14) 0.0279(9) Uani 1 1 d . . . . .
C13 C 0.4746(4) 0.3796(3) 0.41992(14) 0.0320(9) Uani 1 1 d . . . . .
H13 H 0.414302 0.377468 0.393986 0.038 Uiso 1 1 calc R U . . .
C14 C 0.4375(4) 0.3671(3) 0.46924(15) 0.0332(10) Uani 1 1 d . . . . .
H14 H 0.351301 0.358280 0.475878 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6482(4) 0.1396(3) 0.26519(14) 0.0302(9) Uani 1 1 d . . . . .
H15 H 0.707127 0.135084 0.239229 0.036 Uiso 1 1 calc R U . . .
C16 C 0.6913(4) 0.1327(3) 0.31407(14) 0.0305(9) Uani 1 1 d . . . . .
H16 H 0.777873 0.124543 0.320798 0.037 Uiso 1 1 calc R U . . .
C17 C 0.6055(4) 0.1378(3) 0.35340(14) 0.0263(9) Uani 1 1 d . . . . .
C18 C 0.4777(4) 0.1508(3) 0.34057(15) 0.0363(10) Uani 1 1 d . . . . .
H18 H 0.416533 0.154795 0.365706 0.044 Uiso 1 1 calc R U . . .
C19 C 0.4422(4) 0.1576(3) 0.29074(15) 0.0369(10) Uani 1 1 d . . . . .
H19 H 0.356312 0.166200 0.282819 0.044 Uiso 1 1 calc R U . . .
C20 C 0.8106(4) 0.1320(4) 0.47030(15) 0.0443(12) Uani 1 1 d . . . . .
H20 H 0.896563 0.138695 0.478622 0.053 Uiso 1 1 calc R U . . .
C21 C 0.7744(4) 0.1378(4) 0.42058(15) 0.0415(11) Uani 1 1 d . . . . .
H21 H 0.835539 0.147755 0.395859 0.050 Uiso 1 1 calc R U . . .
C22 C 0.6474(4) 0.1288(3) 0.40694(14) 0.0290(9) Uani 1 1 d . . . . .
C23 C 0.5627(4) 0.1117(3) 0.44516(15) 0.0400(11) Uani 1 1 d . . . . .
H23 H 0.476587 0.102890 0.437611 0.048 Uiso 1 1 calc R U . . .
C24 C 0.6039(4) 0.1074(3) 0.49444(15) 0.0396(11) Uani 1 1 d . . . . .
H24 H 0.544171 0.097322 0.519716 0.048 Uiso 1 1 calc R U . . .
N1 N 0.7283(3) 0.3991(2) 0.25612(12) 0.0288(8) Uani 1 1 d . . . . .
N2 N 0.5200(3) 0.3669(3) 0.50805(11) 0.0284(7) Uani 1 1 d . . . . .
N3 N 0.5256(3) 0.1525(2) 0.25326(11) 0.0284(7) Uani 1 1 d . . . . .
N4 N 0.7265(3) 0.1171(3) 0.50738(12) 0.0314(8) Uani 1 1 d . . . . .
O1 O 0.9524(2) 0.4140(2) 0.17612(11) 0.0413(8) Uani 1 1 d . . . . .
O2 O 1.1503(2) 0.4324(2) 0.12426(11) 0.0345(7) Uani 1 1 d . . . . .
O3 O 0.9835(2) 0.3054(2) 0.09867(10) 0.0302(6) Uani 1 1 d . . . . .
O4 O 1.1006(2) 0.1013(2) 0.12142(10) 0.0316(6) Uani 1 1 d . . . . .
O5 O 1.2708(2) 0.2280(2) 0.09826(9) 0.0281(6) Uani 1 1 d . . . . .
O6 O 1.3026(2) 0.1121(2) 0.17239(10) 0.0373(7) Uani 1 1 d . . . . .
O7 O 0.4439(2) 0.4329(2) 0.09156(11) 0.0365(7) Uani 1 1 d . . . . .
O8 O 0.4750(2) 0.3136(2) 0.16418(9) 0.0281(6) Uani 1 1 d . . . . .
O9 O 0.6451(2) 0.4418(2) 0.14344(10) 0.0306(6) Uani 1 1 d . . . . .
O10 O 0.5917(2) 0.1113(2) 0.13410(10) 0.0305(6) Uani 1 1 d . . . . .
O11 O 0.7607(2) 0.2336(2) 0.16325(9) 0.0261(6) Uani 1 1 d . . . . .
O12 O 0.7920(2) 0.1273(2) 0.08491(10) 0.0345(7) Uani 1 1 d . . . . .
O13 O 0.5195(3) 0.2370(3) 0.04740(12) 0.0557(9) Uani 1 1 d . . . . .
H13A H 0.466985 0.207392 0.064768 0.083 Uiso 1 1 calc R U . . .
O14 O 1.2287(3) 0.3119(3) 0.21374(11) 0.0568(10) Uani 1 1 d D . . . .
H14A H 1.285395 0.333600 0.195448 0.085 Uiso 1 1 d DR U . . .
P1 P 1.04741(9) 0.36000(8) 0.14296(4) 0.0303(2) Uani 1 1 d . . . . .
P2 P 1.20584(9) 0.17076(8) 0.14050(4) 0.0267(2) Uani 1 1 d . . . . .
P3 P 0.54078(9) 0.37318(8) 0.12275(4) 0.0264(2) Uani 1 1 d . . . . .
P4 P 0.69762(9) 0.18248(8) 0.11781(4) 0.0254(2) Uani 1 1 d . . . . .
Zn1 Zn 0.77874(4) 0.37619(4) 0.18319(2) 0.02443(11) Uani 1 1 d . . . . .
Zn2 Zn 0.47009(4) 0.16896(4) 0.18089(2) 0.02546(11) Uani 1 1 d . . . . .
Zn3 Zn 0.96825(4) 0.16299(3) 0.07989(2) 0.02460(11) Uani 1 1 d . . . . .
Zn4 Zn 1.27829(4) 0.37317(4) 0.08071(2) 0.02848(12) 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
C1 O13 1.468(4) . ?
C1 C2 1.490(5) . ?
C1 P3 1.838(4) . ?
C1 P4 1.847(4) . ?
C3 O14 1.468(4) . ?
C3 C4 1.493(5) . ?
C3 P2 1.837(4) . ?
C3 P1 1.847(4) . ?
C5 N1 1.333(5) . ?
C5 C6 1.376(5) . ?
C6 C7 1.381(5) . ?
C7 C8 1.384(5) . ?
C7 C12 1.485(5) . ?
C8 C9 1.368(5) . ?
C9 N1 1.342(5) . ?
C10 N2 1.348(5) . ?
C10 C11 1.371(5) . ?
C11 C12 1.389(5) . ?
C12 C13 1.382(5) . ?
C13 C14 1.376(5) . ?
C14 N2 1.337(5) . ?
C15 N3 1.333(5) . ?
C15 C16 1.370(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.390(5) . ?
C17 C22 1.486(5) . ?
C18 C19 1.371(5) . ?
C19 N3 1.330(5) . ?
C20 N4 1.340(5) . ?
C20 C21 1.369(5) . ?
C21 C22 1.382(5) . ?
C22 C23 1.372(6) . ?
C23 C24 1.372(5) . ?
C24 N4 1.335(5) . ?
N1 Zn1 2.030(3) . ?
N2 Zn3 2.022(3) 4_566 ?
N3 Zn2 2.010(3) . ?
N4 Zn4 2.016(3) 4_566 ?
O1 P1 1.512(3) . ?
O1 Zn1 1.899(3) . ?
O2 P1 1.527(3) . ?
O2 Zn4 1.942(3) . ?
O3 P1 1.527(3) . ?
O3 Zn3 1.950(3) . ?
O4 P2 1.517(3) . ?
O4 Zn3 1.942(2) . ?
O5 P2 1.517(3) . ?
O5 Zn4 1.973(3) . ?
O6 P2 1.526(3) . ?
O6 Zn2 1.922(3) 1_655 ?
O7 P3 1.524(3) . ?
O7 Zn4 1.926(3) 1_455 ?
O8 P3 1.520(3) . ?
O8 Zn2 1.961(3) . ?
O9 P3 1.519(3) . ?
O9 Zn1 1.948(2) . ?
O10 P4 1.520(3) . ?
O10 Zn2 1.941(3) . ?
O11 P4 1.525(2) . ?
O11 Zn1 1.963(3) . ?
O12 P4 1.511(3) . ?
O12 Zn3 1.914(2) . ?

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
O13 C1 C2 107.3(3) . . ?
O13 C1 P3 108.6(3) . . ?
C2 C1 P3 110.3(3) . . ?
O13 C1 P4 110.0(3) . . ?
C2 C1 P4 111.2(3) . . ?
P3 C1 P4 109.5(2) . . ?
O14 C3 C4 107.2(3) . . ?
O14 C3 P2 108.9(3) . . ?
C4 C3 P2 110.3(3) . . ?
O14 C3 P1 110.6(3) . . ?
C4 C3 P1 110.8(3) . . ?
P2 C3 P1 109.08(19) . . ?
N1 C5 C6 122.8(4) . . ?
C5 C6 C7 120.1(4) . . ?
C8 C7 C6 116.6(4) . . ?
C8 C7 C12 121.4(4) . . ?
C6 C7 C12 121.9(3) . . ?
C7 C8 C9 120.3(4) . . ?
N1 C9 C8 122.7(4) . . ?
N2 C10 C11 122.4(4) . . ?
C10 C11 C12 120.2(4) . . ?
C13 C12 C11 117.1(4) . . ?
C13 C12 C7 121.8(3) . . ?
C11 C12 C7 121.0(4) . . ?
C14 C13 C12 119.8(4) . . ?
N2 C14 C13 122.9(4) . . ?
N3 C15 C16 122.8(4) . . ?
C15 C16 C17 119.8(4) . . ?
C16 C17 C18 117.0(3) . . ?
C16 C17 C22 121.7(3) . . ?
C18 C17 C22 121.3(4) . . ?
C19 C18 C17 119.8(4) . . ?
N3 C19 C18 122.7(4) . . ?
N4 C20 C21 122.2(4) . . ?
C20 C21 C22 120.4(4) . . ?
C23 C22 C21 116.8(4) . . ?
C23 C22 C17 122.0(3) . . ?
C21 C22 C17 121.3(4) . . ?
C22 C23 C24 120.5(4) . . ?
N4 C24 C23 122.3(4) . . ?
C5 N1 C9 117.3(3) . . ?
C5 N1 Zn1 122.3(3) . . ?
C9 N1 Zn1 120.0(3) . . ?
C14 N2 C10 117.5(3) . . ?
C14 N2 Zn3 123.1(3) . 4_566 ?
C10 N2 Zn3 119.4(3) . 4_566 ?
C19 N3 C15 118.0(3) . . ?
C19 N3 Zn2 121.3(2) . . ?
C15 N3 Zn2 120.7(3) . . ?
C20 N4 C24 117.7(3) . . ?
C20 N4 Zn4 121.5(3) . 4_566 ?
C24 N4 Zn4 120.3(3) . 4_566 ?
P1 O1 Zn1 124.80(16) . . ?
P1 O2 Zn4 115.78(16) . . ?
P1 O3 Zn3 133.27(17) . . ?
P2 O4 Zn3 116.73(16) . . ?
P2 O5 Zn4 132.59(17) . . ?
P2 O6 Zn2 117.99(16) . 1_655 ?
P3 O7 Zn4 117.72(16) . 1_455 ?
P3 O8 Zn2 132.79(17) . . ?
P3 O9 Zn1 116.26(16) . . ?
P4 O10 Zn2 115.11(15) . . ?
P4 O11 Zn1 132.54(16) . . ?
P4 O12 Zn3 124.01(16) . . ?
O3 P1 O1 112.45(15) . . ?
O3 P1 O2 110.65(16) . . ?
O1 P1 O2 111.38(16) . . ?
O3 P1 C3 107.95(17) . . ?
O1 P1 C3 107.80(18) . . ?
O2 P1 C3 106.31(16) . . ?
O5 P2 O4 112.66(15) . . ?
O5 P2 O6 111.12(15) . . ?
O4 P2 O6 110.85(16) . . ?
O5 P2 C3 107.89(17) . . ?
O4 P2 C3 106.70(16) . . ?
O6 P2 C3 107.33(18) . . ?
O9 P3 O8 112.19(15) . . ?
O9 P3 O7 111.23(16) . . ?
O8 P3 O7 110.73(15) . . ?
O9 P3 C1 106.96(16) . . ?
O8 P3 C1 108.04(17) . . ?
O7 P3 C1 107.46(17) . . ?
O12 P4 O10 110.45(16) . . ?
O12 P4 O11 112.74(14) . . ?
O10 P4 O11 111.23(15) . . ?
O12 P4 C1 109.17(17) . . ?
O10 P4 C1 105.35(16) . . ?
O11 P4 C1 107.57(16) . . ?
O1 Zn1 O9 121.05(13) . . ?
O1 Zn1 O11 108.40(11) . . ?
O9 Zn1 O11 102.33(10) . . ?
O1 Zn1 N1 108.22(12) . . ?
O9 Zn1 N1 104.82(12) . . ?
O11 Zn1 N1 111.94(12) . . ?
O6 Zn2 O10 112.14(12) 1_455 . ?
O6 Zn2 O8 112.33(11) 1_455 . ?
O10 Zn2 O8 102.65(11) . . ?
O6 Zn2 N3 109.04(12) 1_455 . ?
O10 Zn2 N3 112.34(12) . . ?
O8 Zn2 N3 108.20(12) . . ?
O12 Zn3 O4 122.94(12) . . ?
O12 Zn3 O3 107.26(11) . . ?
O4 Zn3 O3 101.68(11) . . ?
O12 Zn3 N2 106.55(12) . 4_665 ?
O4 Zn3 N2 104.76(12) . 4_665 ?
O3 Zn3 N2 113.95(12) . 4_665 ?
O7 Zn4 O2 111.92(12) 1_655 . ?
O7 Zn4 O5 113.57(11) 1_655 . ?
O2 Zn4 O5 102.81(11) . . ?
O7 Zn4 N4 110.63(13) 1_655 4_665 ?
O2 Zn4 N4 111.41(13) . 4_665 ?
O5 Zn4 N4 106.14(12) . 4_665 ?

_refine_diff_density_max         0.822
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.083



