# 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. 
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data_mo_nlg-x-70_0ma
_database_code_depnum_ccdc_archive 'CCDC 1544795'
_audit_update_record             
;
2017-09-20 deposited with the CCDC.
2017-09-22 downloaded from the CCDC.
;
_audit_creation_date             2017-09-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H8 N10 O4 Zn, 2(H4 O2)'
_chemical_formula_sum            'H16 N10 O8 Zn'
_chemical_formula_weight         349.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
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      orthorhombic
_space_group_IT_number           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   12.293(4)
_cell_length_b                   17.319(6)
_cell_length_c                   6.536(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1391.5(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2611
_cell_measurement_temperature    205
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1033 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.6603. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2971
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.257
_diffrn_reflns_theta_min         3.315
_diffrn_ambient_temperature      205
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                452
_reflns_number_total             453
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0302
_refine_ls_restrained_S_all      1.198
_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)+(0.0473P)²+1.1970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0707
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H1B(0.5) H1A(0.5)
3.a Free rotating group:
 O2(H2A,H2B)
3.b Rotating group:
 O1(H1B,H1A)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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
Zn1 Zn 0.5000 0.5000 0.5000 0.0153(3) Uani 1 8 d S T P . .
O2 O 0.32095(12) 0.38295(9) 0.0000 0.0250(4) Uani 1 2 d S T P . .
H2A H 0.2548 0.3756 0.0379 0.038 Uiso 0.5 1 d G . . . .
H2B H 0.3551 0.3425 0.0413 0.038 Uiso 0.5 1 d G . . . .
O1 O 0.37744(13) 0.5000 0.2766(3) 0.0295(4) Uani 1 2 d S T P . .
H1B H 0.3701 0.4537 0.2217 0.044 Uiso 0.5 1 d GR . . . .
H1A H 0.3971 0.5277 0.1695 0.044 Uiso 0.5 1 d GR . . . .
N1 N 0.5000 0.37546(13) 0.5000 0.0186(5) Uani 1 4 d S T P . .
N2 N 0.41206(15) 0.33098(11) 0.5000 0.0224(4) Uani 1 2 d S T P . .
N3 N 0.44576(15) 0.25847(11) 0.5000 0.0244(4) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0129(3) 0.0128(3) 0.0204(3) 0.000 0.000 0.000
O2 0.0194(8) 0.0185(8) 0.0371(9) 0.000 0.000 0.0006(6)
O1 0.0327(9) 0.0230(8) 0.0329(9) 0.000 -0.0163(7) 0.000
N1 0.0157(11) 0.0149(12) 0.0253(12) 0.000 0.000 0.000
N2 0.0182(9) 0.0184(9) 0.0307(9) 0.000 0.000 -0.0028(6)
N3 0.0256(10) 0.0167(9) 0.0310(9) 0.000 0.000 -0.0028(7)

_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
Zn1 O1 2.0979(16) . ?
Zn1 O1 2.0979(16) 17_666 ?
Zn1 O1 2.0979(16) 18_556 ?
Zn1 O1 2.0979(16) 2_665 ?
Zn1 N1 2.157(2) . ?
Zn1 N1 2.157(2) 17_666 ?
O2 H2A 0.8599 . ?
O2 H2B 0.8600 . ?
O1 H1B 0.8826 . ?
O1 H1A 0.8821 . ?
N1 N2 1.327(2) . ?
N1 N2 1.327(2) 3_656 ?
N2 N3 1.322(3) . ?
N3 N3 1.333(4) 3_656 ?

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 Zn1 O1 180.0 . 17_666 ?
O1 Zn1 O1 91.80(10) . 2_665 ?
O1 Zn1 O1 88.20(10) 17_666 2_665 ?
O1 Zn1 O1 91.80(10) 17_666 18_556 ?
O1 Zn1 O1 88.20(10) . 18_556 ?
O1 Zn1 O1 180.0 18_556 2_665 ?
O1 Zn1 N1 90.0 18_556 . ?
O1 Zn1 N1 90.0 . . ?
O1 Zn1 N1 90.0 . 17_666 ?
O1 Zn1 N1 90.0 18_556 17_666 ?
O1 Zn1 N1 90.0 2_665 17_666 ?
O1 Zn1 N1 90.0 17_666 . ?
O1 Zn1 N1 90.0 17_666 17_666 ?
O1 Zn1 N1 90.0 2_665 . ?
N1 Zn1 N1 180.0 . 17_666 ?
H2A O2 H2B 104.5 . . ?
Zn1 O1 H1B 110.9 . . ?
Zn1 O1 H1A 110.8 . . ?
H1B O1 H1A 101.4 . . ?
N2 N1 Zn1 125.48(12) 3_656 . ?
N2 N1 Zn1 125.48(12) . . ?
N2 N1 N2 109.0(2) 3_656 . ?
N3 N2 N1 107.22(17) . . ?
N2 N3 N3 108.26(11) . 3_656 ?

_olex2_submission_special_instructions 'No special instructions were received'
