# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 1915361'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'diaquabis(glycinamide)cobalt(II) bromide chloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Br1.052 Cl0.948 Co N4 O4'
_chemical_formula_sum            'C4 H16 Br1.052 Cl0.948 Co N4 O4'
_chemical_formula_weight         360.88

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y+1/2, x, z+1/4'
'-y+1/2, -x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1, x+1/2, z+3/4'
'-y+1, -x+1/2, z+3/4'

_cell_length_a                   11.3708(2)
_cell_length_b                   11.3708(2)
_cell_length_c                   38.3225(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4954.9(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4192
_cell_measurement_theta_min      4.3840
_cell_measurement_theta_max      31.6800

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_F_000             2879
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    4.989
_shelx_estimated_absorpt_T_min   0.189
_shelx_estimated_absorpt_T_max   0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            15188
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         4.254
_diffrn_reflns_theta_max         26.988
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2501
_reflns_number_gt                2324
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.995

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0256P)²+3.9093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2501
_refine_ls_number_parameters     161
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0538
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.031
_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
C11 C 1.0291(4) 0.1701(4) 0.27919(14) 0.0195(10) Uani 1 1 d . . . . .
C21 C 0.9290(4) 0.2538(4) 0.28521(13) 0.0225(10) Uani 1 1 d . . . . .
H21A H 0.8770 0.2222 0.3037 0.027 Uiso 1 1 calc R U . . .
H21B H 0.9602 0.3304 0.2933 0.027 Uiso 1 1 calc R U . . .
C12 C 1.0374(4) 0.1629(4) 0.13966(13) 0.0208(10) Uani 1 1 d . . . . .
C22 C 0.9362(4) 0.2445(4) 0.13200(14) 0.0238(10) Uani 1 1 d . . . . .
H22B H 0.9671 0.3202 0.1231 0.029 Uiso 1 1 calc R U . . .
H22A H 0.8860 0.2095 0.1136 0.029 Uiso 1 1 calc R U . . .
N21 N 0.8608(4) 0.2711(3) 0.25313(10) 0.0212(8) Uani 1 1 d . . . . .
H21D H 0.8421 0.3486 0.2509 0.025 Uiso 1 1 calc R U . . .
H21C H 0.7926 0.2295 0.2545 0.025 Uiso 1 1 calc R U . . .
N11 N 1.0811(4) 0.1248(4) 0.30690(12) 0.0292(10) Uani 1 1 d . . . . .
H11A H 1.1413 0.0770 0.3043 0.035 Uiso 1 1 calc R U . . .
H11B H 1.0555 0.1425 0.3279 0.035 Uiso 1 1 calc R U . . .
N22 N 0.8650(4) 0.2663(3) 0.16334(10) 0.0215(8) Uani 1 1 d . . . . .
H22C H 0.7966 0.2250 0.1619 0.026 Uiso 1 1 calc R U . . .
H22D H 0.8467 0.3441 0.1646 0.026 Uiso 1 1 calc R U . . .
N12 N 1.0958(4) 0.1196(4) 0.11321(12) 0.0310(10) Uani 1 1 d . . . . .
H12A H 1.1554 0.0719 0.1169 0.037 Uiso 1 1 calc R U . . .
H12B H 1.0754 0.1383 0.0918 0.037 Uiso 1 1 calc R U . . .
O1W O 0.8566(3) 0.0576(2) 0.20915(12) 0.0227(6) Uani 1 1 d D . . . .
O2W O 1.0599(3) 0.3682(3) 0.20844(12) 0.0321(7) Uani 1 1 d D . . . .
O11 O 1.0628(3) 0.1473(3) 0.24904(9) 0.0238(7) Uani 1 1 d . . . . .
O12 O 1.0630(3) 0.1390(3) 0.17042(9) 0.0244(7) Uani 1 1 d . . . . .
Co1 Co 0.95762(4) 0.21556(4) 0.20895(4) 0.01850(17) Uani 1 1 d . . . . .
Br1 Br 1.0475(6) 0.1885(6) 0.0315(2) 0.0215(3) Uani 0.508(5) 1 d . U P A 1
Cl1 Cl 1.0477(15) 0.1910(16) 0.0301(6) 0.0215(3) Uani 0.492(5) 1 d . U P A 2
Br2 Br 1.1761(6) 0.4485(6) 0.13413(19) 0.0226(3) Uani 0.544(5) 1 d . U P . .
Cl2 Cl 1.1803(18) 0.4489(17) 0.1336(6) 0.0226(3) Uani 0.456(5) 1 d . U P B 2
H2WA H 1.100(4) 0.390(4) 0.1911(9) 0.022(13) Uiso 1 1 d D . . . .
H2WB H 1.077(7) 0.409(6) 0.2263(11) 0.10(3) Uiso 1 1 d D . . . .
H1WA H 0.869(7) 0.008(4) 0.1931(10) 0.05(2) Uiso 1 1 d D . . . .
H1WB H 0.853(6) 0.025(5) 0.2289(7) 0.05(2) Uiso 1 1 d 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
C11 O11 1.245(6) . ?
C11 N11 1.320(6) . ?
C11 C21 1.502(7) . ?
C21 N21 1.467(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C12 O12 1.244(6) . ?
C12 N12 1.308(6) . ?
C12 C22 1.507(6) . ?
C22 N22 1.470(6) . ?
C22 H22B 0.9900 . ?
C22 H22A 0.9900 . ?
N21 Co1 2.116(4) . ?
N21 H21D 0.9100 . ?
N21 H21C 0.9100 . ?
N11 H11A 0.8800 . ?
N11 H11B 0.8800 . ?
N22 Co1 2.121(4) . ?
N22 H22C 0.9100 . ?
N22 H22D 0.9100 . ?
N12 H12A 0.8800 . ?
N12 H12B 0.8800 . ?
O1W Co1 2.132(3) . ?
O1W H1WA 0.845(14) . ?
O1W H1WB 0.847(14) . ?
O2W Co1 2.089(3) . ?
O2W H2WA 0.840(14) . ?
O2W H2WB 0.844(14) . ?
O11 Co1 2.096(3) . ?
O12 Co1 2.091(3) . ?

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
O11 C11 N11 121.9(5) . . ?
O11 C11 C21 120.5(4) . . ?
N11 C11 C21 117.6(4) . . ?
N21 C21 C11 110.9(4) . . ?
N21 C21 H21A 109.5 . . ?
C11 C21 H21A 109.5 . . ?
N21 C21 H21B 109.5 . . ?
C11 C21 H21B 109.5 . . ?
H21A C21 H21B 108.0 . . ?
O12 C12 N12 122.3(5) . . ?
O12 C12 C22 119.8(4) . . ?
N12 C12 C22 117.9(4) . . ?
N22 C22 C12 111.4(4) . . ?
N22 C22 H22B 109.3 . . ?
C12 C22 H22B 109.3 . . ?
N22 C22 H22A 109.3 . . ?
C12 C22 H22A 109.3 . . ?
H22B C22 H22A 108.0 . . ?
C21 N21 Co1 110.8(3) . . ?
C21 N21 H21D 109.5 . . ?
Co1 N21 H21D 109.5 . . ?
C21 N21 H21C 109.5 . . ?
Co1 N21 H21C 109.5 . . ?
H21D N21 H21C 108.1 . . ?
C11 N11 H11A 120.0 . . ?
C11 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C22 N22 Co1 110.7(3) . . ?
C22 N22 H22C 109.5 . . ?
Co1 N22 H22C 109.5 . . ?
C22 N22 H22D 109.5 . . ?
Co1 N22 H22D 109.5 . . ?
H22C N22 H22D 108.1 . . ?
C12 N12 H12A 120.0 . . ?
C12 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
Co1 O1W H1WA 118(5) . . ?
Co1 O1W H1WB 114(5) . . ?
H1WA O1W H1WB 112(3) . . ?
Co1 O2W H2WA 123(4) . . ?
Co1 O2W H2WB 125(5) . . ?
H2WA O2W H2WB 111(3) . . ?
C11 O11 Co1 115.3(3) . . ?
C12 O12 Co1 116.4(3) . . ?
O2W Co1 O12 91.16(14) . . ?
O2W Co1 O11 89.82(15) . . ?
O12 Co1 O11 92.09(11) . . ?
O2W Co1 N21 92.81(16) . . ?
O12 Co1 N21 170.86(14) . . ?
O11 Co1 N21 79.69(14) . . ?
O2W Co1 N22 92.44(16) . . ?
O12 Co1 N22 79.39(14) . . ?
O11 Co1 N22 171.22(14) . . ?
N21 Co1 N22 108.64(12) . . ?
O2W Co1 O1W 178.73(13) . . ?
O12 Co1 O1W 87.73(14) . . ?
O11 Co1 O1W 89.58(14) . . ?
N21 Co1 O1W 88.19(15) . . ?
N22 Co1 O1W 87.98(15) . . ?

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
O11 C11 C21 N21 17.1(6) . . . . ?
N11 C11 C21 N21 -164.6(4) . . . . ?
O12 C12 C22 N22 -11.8(6) . . . . ?
N12 C12 C22 N22 168.3(4) . . . . ?
C11 C21 N21 Co1 -17.3(5) . . . . ?
C12 C22 N22 Co1 16.1(4) . . . . ?
N11 C11 O11 Co1 174.3(4) . . . . ?
C21 C11 O11 Co1 -7.4(6) . . . . ?
N12 C12 O12 Co1 -179.3(4) . . . . ?
C22 C12 O12 Co1 0.9(5) . . . . ?

_refine_diff_density_max         0.307
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.063


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1c_LT
_database_code_depnum_ccdc_archive 'CCDC 1915362'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'diaquabis(glycinamide)nickel(II) iodide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Co N4 O4, I2'
_chemical_formula_sum            'C4 H16 Co I2 N4 O4'
_chemical_formula_weight         496.94

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'
Co Co 0.3494 0.9721 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   7.3966(4)
_cell_length_b                   19.1784(8)
_cell_length_c                   10.1512(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1440.00(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1430
_cell_measurement_theta_min      4.5250
_cell_measurement_theta_max      31.1990

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_F_000             932
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    5.482
_shelx_estimated_absorpt_T_min   0.474
_shelx_estimated_absorpt_T_max   0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.18b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            4648
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.251
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1606
_reflns_number_gt                1211
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2018)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0155P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1606
_refine_ls_number_parameters     81
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0529
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_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
H1W H 0.311(6) 0.2870(16) 0.504(5) 0.041(17) Uiso 1 1 d D . . . .
H2W H 0.965(7) 0.284(2) 0.354(5) 0.09(3) Uiso 1 1 d D . . . .
I1 I 0.15242(5) 0.40052(2) 0.59961(3) 0.02531(12) Uani 1 1 d . . . . .
Co1 Co 0.63188(13) 0.2500 0.43367(9) 0.0187(2) Uani 1 2 d S T P . .
C1 C 0.6252(6) 0.3916(2) 0.3334(5) 0.0203(11) Uani 1 1 d . . . . .
O2W O 0.9109(7) 0.2500 0.3908(5) 0.0233(11) Uani 1 2 d DS T P . .
O1 O 0.5933(4) 0.33076(17) 0.2950(3) 0.0247(8) Uani 1 1 d . . . . .
O1W O 0.3557(8) 0.2500 0.4710(6) 0.0376(14) Uani 1 2 d DS T P . .
N2 N 0.6777(5) 0.3394(2) 0.5523(4) 0.0235(10) Uani 1 1 d . . . . .
H2C H 0.5984 0.3392 0.6208 0.028 Uiso 1 1 calc R U . . .
H2D H 0.7914 0.3373 0.5863 0.028 Uiso 1 1 calc R U . . .
C2 C 0.6572(7) 0.4049(3) 0.4783(4) 0.0229(11) Uani 1 1 d . . . . .
H2B H 0.7677 0.4334 0.4891 0.027 Uiso 1 1 calc R U . . .
H2A H 0.5541 0.4316 0.5148 0.027 Uiso 1 1 calc R U . . .
N1 N 0.6270(5) 0.4452(2) 0.2548(4) 0.0304(11) Uani 1 1 d . . . . .
H1A H 0.6052 0.4396 0.1702 0.036 Uiso 1 1 calc R U . . .
H1B H 0.6501 0.4870 0.2862 0.036 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
Co1 O1W 2.078(6) . ?
Co1 O2W 2.109(5) . ?
Co1 O1 2.113(3) 7_565 ?
Co1 O1 2.113(3) . ?
Co1 N2 2.122(4) 7_565 ?
Co1 N2 2.122(4) . ?
C1 O1 1.252(5) . ?
C1 N1 1.301(6) . ?
C1 C2 1.512(6) . ?
N2 C2 1.471(6) . ?

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
O1W Co1 O2W 178.6(2) . . ?
O1W Co1 O1 89.35(15) . 7_565 ?
O2W Co1 O1 89.69(13) . 7_565 ?
O1W Co1 O1 89.35(15) . . ?
O2W Co1 O1 89.69(13) . . ?
O1 Co1 O1 94.31(18) 7_565 . ?
O1W Co1 N2 93.08(15) . 7_565 ?
O2W Co1 N2 87.75(14) . 7_565 ?
O1 Co1 N2 78.90(14) 7_565 7_565 ?
O1 Co1 N2 172.74(14) . 7_565 ?
O1W Co1 N2 93.08(15) . . ?
O2W Co1 N2 87.75(14) . . ?
O1 Co1 N2 172.74(14) 7_565 . ?
O1 Co1 N2 78.89(14) . . ?
N2 Co1 N2 107.8(2) 7_565 . ?
O1 C1 N1 123.2(5) . . ?
O1 C1 C2 119.3(4) . . ?
N1 C1 C2 117.5(4) . . ?
C1 O1 Co1 116.7(3) . . ?
C2 N2 Co1 112.6(3) . . ?
N2 C2 C1 111.6(4) . . ?

_refine_diff_density_max         0.940
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.161


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1915369'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'diaquabis(glycinamide)nickel(II) bromide chloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 N4 Ni O4, Br0.937 Cl1.063 '
_chemical_formula_sum            'C4 H16 Br0.937 Cl1.063 N4 Ni O4'
_chemical_formula_weight         355.61

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   11.3175(3)
_cell_length_b                   11.3175(3)
_cell_length_c                   38.0842(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4878.0(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4303
_cell_measurement_theta_min      4.1280
_cell_measurement_theta_max      31.4850

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_F_000             2863
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.330
_exptl_absorpt_coefficient_mu    4.905
_shelx_estimated_absorpt_T_min   0.177
_shelx_estimated_absorpt_T_max   0.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            11070
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         4.281
_diffrn_reflns_theta_max         26.985
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2662
_reflns_number_gt                2499
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.994

_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2014)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2014)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0237P)²+0.0116P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.470(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2662
_refine_ls_number_parameters     161
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0485
_refine_ls_wR_factor_gt          0.0474
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.101
_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
H1WB H 0.599(6) 0.577(5) 0.1939(10) 0.06(2) Uiso 1 1 d D . . . .
H2WA H 0.967(5) 0.353(6) 0.2342(8) 0.042(17) Uiso 1 1 d D . . . .
H2WB H 0.990(5) 0.368(6) 0.1980(12) 0.06(2) Uiso 1 1 d D . . . .
H1WA H 0.613(5) 0.603(4) 0.2287(10) 0.029(15) Uiso 1 1 d D . . . .
Ni1 Ni 0.78486(4) 0.45782(4) 0.21330(5) 0.01532(15) Uani 1 1 d . . . . .
O2W O 0.9407(2) 0.3555(2) 0.21356(11) 0.0182(5) Uani 1 1 d D . . . .
O11 O 0.8598(3) 0.5622(3) 0.17578(9) 0.0198(7) Uani 1 1 d . . . . .
O12 O 0.8520(3) 0.5618(3) 0.25260(9) 0.0211(7) Uani 1 1 d . . . . .
C22 C 0.7428(4) 0.4277(4) 0.28880(12) 0.0185(9) Uani 1 1 d . . . . .
H22B H 0.7738 0.3749 0.3073 0.022 Uiso 1 1 calc R U . . .
H22A H 0.6659 0.4595 0.2968 0.022 Uiso 1 1 calc R U . . .
O1W O 0.6309(3) 0.5584(2) 0.21290(12) 0.0295(7) Uani 1 1 d D . . . .
N22 N 0.7262(3) 0.3604(3) 0.25611(10) 0.0182(7) Uani 1 1 d . . . . .
H22C H 0.6483 0.3428 0.2533 0.022 Uiso 1 1 calc R U . . .
H22D H 0.7671 0.2913 0.2574 0.022 Uiso 1 1 calc R U . . .
C21 C 0.7521(4) 0.4342(4) 0.13778(13) 0.0212(9) Uani 1 1 d . . . . .
H21A H 0.6757 0.4654 0.1291 0.025 Uiso 1 1 calc R U . . .
H21B H 0.7859 0.3830 0.1192 0.025 Uiso 1 1 calc R U . . .
C11 C 0.8347(4) 0.5352(4) 0.14479(13) 0.0175(9) Uani 1 1 d . . . . .
C12 C 0.8276(4) 0.5276(4) 0.28287(13) 0.0169(9) Uani 1 1 d . . . . .
N21 N 0.7319(3) 0.3643(3) 0.16939(10) 0.0179(7) Uani 1 1 d . . . . .
H21D H 0.7733 0.2955 0.1680 0.022 Uiso 1 1 calc R U . . .
H21C H 0.6538 0.3462 0.1712 0.022 Uiso 1 1 calc R U . . .
N11 N 0.8780(4) 0.5943(4) 0.11816(11) 0.0260(9) Uani 1 1 d . . . . .
H11A H 0.9257 0.6545 0.1219 0.031 Uiso 1 1 calc R U . . .
H11B H 0.8593 0.5740 0.0966 0.031 Uiso 1 1 calc R U . . .
N12 N 0.8734(3) 0.5797(4) 0.31078(11) 0.0236(9) Uani 1 1 d . . . . .
H12A H 0.9221 0.6397 0.3082 0.028 Uiso 1 1 calc R U . . .
H12B H 0.8553 0.5544 0.3320 0.028 Uiso 1 1 calc R U . . .
Br2 Br 1.0522(9) 0.8125(9) 0.2865(3) 0.0151(9) Uani 0.413(5) 1 d . U P A 1
Cl2 Cl 1.0422(16) 0.7995(16) 0.2838(5) 0.0151(9) Uani 0.587(5) 1 d . U P A 2
Br1 Br 1.0533(13) 0.8212(13) 0.1374(4) 0.0194(7) Uani 0.524(5) 1 d . U P B 1
Cl1 Cl 1.049(3) 0.818(3) 0.1390(12) 0.0194(7) Uani 0.476(5) 1 d . U P B 2


_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
Ni1 O11 2.039(3) . ?
Ni1 O12 2.050(3) . ?
Ni1 N21 2.068(3) . ?
Ni1 N22 2.077(3) . ?
Ni1 O1W 2.081(3) . ?
Ni1 O2W 2.109(3) . ?
O11 C11 1.252(5) . ?
O12 C12 1.247(5) . ?
C22 N22 1.472(5) . ?
C22 C12 1.499(7) . ?
C21 N21 1.458(6) . ?
C21 C11 1.501(6) . ?
C11 N11 1.310(6) . ?
C12 N12 1.322(6) . ?

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
O11 Ni1 O12 91.42(10) . . ?
O11 Ni1 N21 81.40(13) . . ?
O12 Ni1 N21 172.61(13) . . ?
O11 Ni1 N22 172.16(13) . . ?
O12 Ni1 N22 81.39(13) . . ?
N21 Ni1 N22 105.68(11) . . ?
O11 Ni1 O1W 91.49(13) . . ?
O12 Ni1 O1W 90.08(14) . . ?
N21 Ni1 O1W 91.82(15) . . ?
N22 Ni1 O1W 91.64(15) . . ?
O11 Ni1 O2W 88.48(13) . . ?
O12 Ni1 O2W 90.10(13) . . ?
N21 Ni1 O2W 87.99(13) . . ?
N22 Ni1 O2W 88.41(14) . . ?
O1W Ni1 O2W 179.82(16) . . ?
C11 O11 Ni1 115.1(3) . . ?
C12 O12 Ni1 114.5(3) . . ?
N22 C22 C12 110.2(4) . . ?
C22 N22 Ni1 110.4(3) . . ?
N21 C21 C11 111.3(4) . . ?
O11 C11 N11 121.3(4) . . ?
O11 C11 C21 119.7(4) . . ?
N11 C11 C21 119.0(4) . . ?
O12 C12 N12 121.2(4) . . ?
O12 C12 C22 121.0(4) . . ?
N12 C12 C22 117.8(4) . . ?
C21 N21 Ni1 110.2(3) . . ?

_refine_diff_density_max         0.385
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.058


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1915365'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_3c                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note
RESPONSE: These reflections were cut off by the beamstop.
;
# Added during the CSD deposition process: Friday 10 May 2019 06:42 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 Cu1 N4 O2, Cu1 I3'
_chemical_formula_sum            'C4 H12 Cu2 I3 N4 O2'
_chemical_formula_weight         655.96

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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 '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      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                   8.0185(4)
_cell_length_b                   8.6901(4)
_cell_length_c                   11.0929(5)
_cell_angle_alpha                84.575(4)
_cell_angle_beta                 77.367(4)
_cell_angle_gamma                72.679(4)
_cell_volume                     719.69(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4212
_cell_measurement_theta_min      4.7390
_cell_measurement_theta_max      32.3130

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.027
_exptl_crystal_F_000             594
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    9.378
_shelx_estimated_absorpt_T_min   0.138
_shelx_estimated_absorpt_T_max   0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.26403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            7861
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.180
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3084
_reflns_number_gt                2548
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;

_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2016/4 (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)+(0.0353P)²+2.0974P] 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       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3084
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_restrained_S_all      0.843
_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
C101 C 0.5338(7) -0.2278(7) 0.1056(5) 0.0407(13) Uani 1 1 d . . . . .
C102 C 0.5425(7) -0.3440(7) 0.2163(5) 0.0455(14) Uani 1 1 d . . . . .
H106 H 0.4259 -0.3591 0.2496 0.055 Uiso 1 1 calc R U . . .
H105 H 0.6255 -0.4479 0.1919 0.055 Uiso 1 1 calc R U . . .
C103 C 0.9623(7) 0.0650(6) 0.1839(5) 0.0368(12) Uani 1 1 d . . . . .
C104 C 0.9983(8) -0.0189(6) 0.3039(5) 0.0401(12) Uani 1 1 d . . . . .
H103 H 1.1093 -0.1050 0.2895 0.048 Uiso 1 1 calc R U . . .
H104 H 1.0085 0.0567 0.3590 0.048 Uiso 1 1 calc R U . . .
O11 O 0.6285(5) -0.1336(5) 0.0883(3) 0.0451(10) Uani 1 1 d . . . . .
O21 O 0.8533(5) 0.0305(5) 0.1313(3) 0.0400(9) Uani 1 1 d . . . . .
N11 N 0.4325(7) -0.2325(7) 0.0307(5) 0.0643(17) Uani 1 1 d . . . . .
H11A H 0.4288 -0.1693 -0.0338 0.077 Uiso 1 1 calc R U . . .
H11B H 0.3690 -0.2988 0.0453 0.077 Uiso 1 1 calc R U . . .
N101 N 0.6021(6) -0.2764(6) 0.3105(4) 0.0419(11) Uani 1 1 d . . . . .
H108 H 0.6701 -0.3554 0.3506 0.050 Uiso 1 1 calc R U . . .
H107 H 0.5082 -0.2234 0.3650 0.050 Uiso 1 1 calc R U . . .
N102 N 1.0513(7) 0.1652(6) 0.1351(5) 0.0541(14) Uani 1 1 d . . . . .
H101 H 1.0376 0.2112 0.0644 0.065 Uiso 1 1 calc R U . . .
H102 H 1.1241 0.1858 0.1734 0.065 Uiso 1 1 calc R U . . .
N22 N 0.8490(6) -0.0856(6) 0.3600(4) 0.0405(11) Uani 1 1 d . . . . .
H22C H 0.7680 -0.0160 0.4123 0.049 Uiso 1 1 calc R U . . .
H22D H 0.8885 -0.1771 0.4018 0.049 Uiso 1 1 calc R U . . .
Cu1 Cu 0.74070(9) -0.12646(9) 0.22635(6) 0.04159(18) Uani 1 1 d . . . . .
Cu2 Cu 0.12297(10) 0.43898(9) 0.36934(7) 0.0496(2) Uani 1 1 d . . . . .
I1 I 0.08127(4) 0.57732(4) 0.15092(3) 0.03569(11) Uani 1 1 d . . . . .
I2 I -0.18519(4) 0.36989(4) 0.48163(3) 0.03481(11) Uani 1 1 d . . . . .
I3 I 0.39021(5) 0.17243(4) 0.33524(4) 0.04462(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
C101 O11 1.249(7) . ?
C101 N11 1.293(7) . ?
C101 C102 1.515(7) . ?
C102 N101 1.471(8) . ?
C102 H106 0.9700 . ?
C102 H105 0.9700 . ?
C103 O21 1.267(6) . ?
C103 N102 1.293(7) . ?
C103 C104 1.499(7) . ?
C104 N22 1.474(7) . ?
C104 H103 0.9700 . ?
C104 H104 0.9700 . ?
O11 Cu1 1.953(4) . ?
O21 Cu1 1.958(4) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N101 Cu1 1.996(4) . ?
N101 H108 0.8900 . ?
N101 H107 0.8900 . ?
N102 H101 0.8600 . ?
N102 H102 0.8600 . ?
N22 Cu1 1.981(4) . ?
N22 H22C 0.8900 . ?
N22 H22D 0.8900 . ?
Cu2 I3 2.6374(8) . ?
Cu2 I1 2.6443(8) . ?
Cu2 I2 2.6671(9) 2_566 ?
Cu2 I2 2.7228(9) . ?
I2 Cu2 2.6671(9) 2_566 ?

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
O11 C101 N11 122.4(5) . . ?
O11 C101 C102 118.6(5) . . ?
N11 C101 C102 119.0(5) . . ?
N101 C102 C101 108.5(4) . . ?
N101 C102 H106 110.0 . . ?
C101 C102 H106 110.0 . . ?
N101 C102 H105 110.0 . . ?
C101 C102 H105 110.0 . . ?
H106 C102 H105 108.4 . . ?
O21 C103 N102 122.5(5) . . ?
O21 C103 C104 119.5(5) . . ?
N102 C103 C104 118.0(5) . . ?
N22 C104 C103 108.2(4) . . ?
N22 C104 H103 110.1 . . ?
C103 C104 H103 110.1 . . ?
N22 C104 H104 110.1 . . ?
C103 C104 H104 110.1 . . ?
H103 C104 H104 108.4 . . ?
C101 O11 Cu1 114.4(3) . . ?
C103 O21 Cu1 113.2(3) . . ?
C101 N11 H11A 120.0 . . ?
C101 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C102 N101 Cu1 108.6(3) . . ?
C102 N101 H108 110.0 . . ?
Cu1 N101 H108 110.0 . . ?
C102 N101 H107 110.0 . . ?
Cu1 N101 H107 110.0 . . ?
H108 N101 H107 108.4 . . ?
C103 N102 H101 120.0 . . ?
C103 N102 H102 120.0 . . ?
H101 N102 H102 120.0 . . ?
C104 N22 Cu1 108.6(3) . . ?
C104 N22 H22C 110.0 . . ?
Cu1 N22 H22C 110.0 . . ?
C104 N22 H22D 110.0 . . ?
Cu1 N22 H22D 110.0 . . ?
H22C N22 H22D 108.4 . . ?
O11 Cu1 O21 89.25(15) . . ?
O11 Cu1 N22 171.69(18) . . ?
O21 Cu1 N22 84.05(17) . . ?
O11 Cu1 N101 84.21(17) . . ?
O21 Cu1 N101 172.74(16) . . ?
N22 Cu1 N101 102.18(19) . . ?
I3 Cu2 I1 108.45(3) . . ?
I3 Cu2 I2 109.74(3) . 2_566 ?
I1 Cu2 I2 112.86(3) . 2_566 ?
I3 Cu2 I2 110.52(3) . . ?
I1 Cu2 I2 108.13(3) . . ?
I2 Cu2 I2 107.12(3) 2_566 . ?
Cu2 I2 Cu2 72.88(3) 2_566 . ?

_refine_diff_density_max         1.084
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.182


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1915366'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'glycinamide hydrochloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H7 N2 O, Cl'
_chemical_formula_sum            'C2 H7 Cl N2 O'
_chemical_formula_weight         110.55

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'
Cl Cl 0.1484 0.1585 '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                   4.6688(9)
_cell_length_b                   6.2057(13)
_cell_length_c                   8.898(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.486(19)
_cell_angle_gamma                90
_cell_volume                     252.65(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    425
_cell_measurement_theta_min      4.6600
_cell_measurement_theta_max      31.6830

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_F_000             116
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.770
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.615
_shelx_estimated_absorpt_T_min   0.649
_shelx_estimated_absorpt_T_max   0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            1268
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.600
_diffrn_reflns_theta_max         25.987
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             543
_reflns_number_gt                464
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0579P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         543
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.002
_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
H1A H 0.528(7) 0.2500 0.470(4) 0.029(8) Uiso 1 2 d S . P . .
H1B H 0.224(8) 0.2500 0.373(4) 0.042(9) Uiso 1 2 d S . P . .
H2B H 0.454(10) 0.2500 0.965(6) 0.071(13) Uiso 1 2 d S . P . .
H2C H 0.186(5) 0.136(4) 0.869(3) 0.051(7) Uiso 1 1 d . . . . .
H2A H 0.571(5) 0.120(4) 0.751(3) 0.049(6) Uiso 1 1 d . . . . .
Cl1 Cl 0.87799(15) 0.2500 0.12754(9) 0.0410(3) Uani 1 2 d S T P . .
N2 N 0.3004(6) 0.2500 0.8706(3) 0.0326(6) Uani 1 2 d S T P . .
C2 C 0.4523(6) 0.2500 0.7400(4) 0.0345(7) Uani 1 2 d S T P . .
O1 O -0.0286(4) 0.2500 0.5908(3) 0.0429(6) Uani 1 2 d S T P . .
N1 N 0.3454(5) 0.2500 0.4649(3) 0.0338(6) Uani 1 2 d S T P . .
C1 C 0.2336(5) 0.2500 0.5899(3) 0.0286(6) Uani 1 2 d S 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
N2 C2 1.477(4) . ?
C2 C1 1.511(4) . ?
O1 C1 1.226(3) . ?
N1 C1 1.319(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
N2 C2 C1 110.4(2) . . ?
O1 C1 N1 124.7(3) . . ?
O1 C1 C2 119.6(3) . . ?
N1 C1 C2 115.7(2) . . ?

_refine_diff_density_max         0.241
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.072


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_GLyamHI
_database_code_depnum_ccdc_archive 'CCDC 1915367'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '2-aminoacetamide hydroiodide'
_chemical_name_common            'glycinamide hydroiodide'
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H7 N2 O, I'
_chemical_formula_sum            'C2 H7 I N2 O'
_chemical_formula_weight         202.00

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'

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

_cell_length_a                   4.68800(10)
_cell_length_b                   18.6082(4)
_cell_length_c                   6.7363(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     587.64(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2585
_cell_measurement_theta_min      4.4960
_cell_measurement_theta_max      31.0030

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    5.329
_shelx_estimated_absorpt_T_min   0.483
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            4855
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.347
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             929
_reflns_number_gt                810
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2018)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0195P)²+0.0168P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         929
_refine_ls_number_parameters     44
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0188
_refine_ls_wR_factor_ref         0.0430
_refine_ls_wR_factor_gt          0.0409
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_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
N2 N 1.0983(6) 0.42509(13) 0.2500 0.0364(6) Uani 1 2 d DS T P . .
N1 N 0.8975(5) 0.23536(14) 0.2500 0.0405(6) Uani 1 2 d S T P . .
H1A H 0.9769 0.1937 0.2500 0.049 Uiso 1 2 calc R U P . .
H1B H 0.7146 0.2389 0.2500 0.049 Uiso 1 2 calc R U P . .
O1 O 1.3181(5) 0.29504(12) 0.2500 0.0527(7) Uani 1 2 d S T P . .
C2 C 0.8965(6) 0.36479(16) 0.2500 0.0345(6) Uani 1 2 d S T P . .
H2A H 0.7757 0.3675 0.1334 0.041 Uiso 0.5 1 calc R U P . .
H2B H 0.7757 0.3675 0.3666 0.041 Uiso 0.5 1 calc R U P . .
H2C H 1.220(6) 0.4246(12) 0.143(3) 0.063(9) Uiso 1 1 d D . . . .
H2D H 1.003(8) 0.4680(12) 0.2500 0.057(10) Uiso 1 2 d DS . P . .
I1 I 0.38862(4) 0.07337(2) 0.2500 0.03726(8) Uani 1 2 d S T P . .
C1 C 1.0573(7) 0.29425(16) 0.2500 0.0330(7) Uani 1 2 d S 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
N2 C2 1.468(4) . ?
N1 C1 1.327(4) . ?
O1 C1 1.223(4) . ?
C2 C1 1.514(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
N2 C2 C1 110.0(2) . . ?
O1 C1 N1 125.0(3) . . ?
O1 C1 C2 119.2(3) . . ?
N1 C1 C2 115.8(3) . . ?

_refine_diff_density_max         0.595
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.087


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_2c_RT
_database_code_depnum_ccdc_archive 'CCDC 1915363'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'diaquabis(glycinamide)nickel(II) iodide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 N4 Ni O4, I2'
_chemical_formula_sum            'C4 H16 I2 N4 Ni O4'
_chemical_formula_weight         496.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ni Ni 0.3393 1.1124 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   7.5456(3)
_cell_length_b                   18.9706(7)
_cell_length_c                   10.1902(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1458.67(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2423
_cell_measurement_theta_min      4.9280
_cell_measurement_theta_max      29.9900

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    5.565
_shelx_estimated_absorpt_T_min   0.305
_shelx_estimated_absorpt_T_max   0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            5770
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.297
_diffrn_reflns_theta_max         26.988
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1626
_reflns_number_gt                1374
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2018)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0254P)²+1.6186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1626
_refine_ls_number_parameters     81
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0698
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.003
_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
H2W H 0.322(10) 0.711(2) 1.031(8) 0.18(4) Uiso 1 1 d D . . . .
H1W H 0.976(10) 0.718(3) 1.137(7) 0.21(5) Uiso 1 1 d D . . . .
Ni1 Ni 0.64379(10) 0.7500 1.06848(7) 0.04045(19) Uani 1 2 d S T P . .
C1 C 0.6398(5) 0.6111(2) 1.1663(4) 0.0448(10) Uani 1 1 d . . . . .
O1W O 0.9187(7) 0.7500 1.0965(5) 0.0641(13) Uani 1 2 d DS T P . .
N2 N 0.6710(6) 0.6628(2) 0.9478(3) 0.0613(11) Uani 1 1 d . . . . .
H2C H 0.5852 0.6630 0.8879 0.074 Uiso 1 1 calc R U . . .
H2D H 0.7744 0.6651 0.9060 0.074 Uiso 1 1 calc R U . . .
N1 N 0.6391(5) 0.5565(2) 1.2459(4) 0.0697(12) Uani 1 1 d . . . . .
H1A H 0.6247 0.5627 1.3288 0.084 Uiso 1 1 calc R U . . .
H1B H 0.6530 0.5147 1.2150 0.084 Uiso 1 1 calc R U . . .
C2 C 0.6628(6) 0.5979(2) 1.0222(4) 0.0508(11) Uani 1 1 d . . . . .
H2B H 0.7709 0.5713 1.0081 0.061 Uiso 1 1 calc R U . . .
H2A H 0.5644 0.5696 0.9906 0.061 Uiso 1 1 calc R U . . .
O1 O 0.6200(5) 0.67270(16) 1.2074(3) 0.0615(9) Uani 1 1 d . . . . .
O2W O 0.3691(8) 0.7500 1.0547(8) 0.0871(18) Uani 1 2 d DS T P . .
I1 I 0.15677(4) 0.60206(2) 0.89955(3) 0.05401(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
Ni1 O1 2.046(3) 7_575 ?
Ni1 O1 2.046(3) . ?
Ni1 N2 2.071(4) 7_575 ?
Ni1 N2 2.071(4) . ?
Ni1 O2W 2.078(6) . ?
Ni1 O1W 2.094(5) . ?
C1 O1 1.251(5) . ?
C1 N1 1.314(6) . ?
C1 C2 1.500(6) . ?
N2 C2 1.448(5) . ?

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 Ni1 O1 91.57(17) 7_575 . ?
O1 Ni1 N2 81.19(14) 7_575 7_575 ?
O1 Ni1 N2 172.64(13) . 7_575 ?
O1 Ni1 N2 172.64(13) 7_575 . ?
O1 Ni1 N2 81.19(14) . . ?
N2 Ni1 N2 106.0(2) 7_575 . ?
O1 Ni1 O2W 87.67(19) 7_575 . ?
O1 Ni1 O2W 87.67(19) . . ?
N2 Ni1 O2W 93.37(18) 7_575 . ?
N2 Ni1 O2W 93.37(19) . . ?
O1 Ni1 O1W 89.57(14) 7_575 . ?
O1 Ni1 O1W 89.57(14) . . ?
N2 Ni1 O1W 89.00(15) 7_575 . ?
N2 Ni1 O1W 89.00(15) . . ?
O2W Ni1 O1W 176.0(3) . . ?
O1 C1 N1 121.9(4) . . ?
O1 C1 C2 119.8(4) . . ?
N1 C1 C2 118.3(4) . . ?
C2 N2 Ni1 111.4(3) . . ?
N2 C2 C1 112.1(3) . . ?
C1 O1 Ni1 115.4(3) . . ?

_refine_diff_density_max         0.921
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.087


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1915372'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 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         'C4 H12 1.30(Br1) 0.70(Cl1) Cu N4 O2'
_chemical_formula_sum            'C4 H12 1.30(Br1) 0.70(Cl1) Cu N4 O2'
_chemical_formula_weight         340.41

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   7.0098(5)
_cell_length_b                   7.8128(3)
_cell_length_c                   9.4100(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.963(6)
_cell_angle_gamma                90
_cell_volume                     504.16(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1932
_cell_measurement_theta_min      4.8330
_cell_measurement_theta_max      32.7430

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_F_000             333
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    7.478
_shelx_estimated_absorpt_T_min   0.098
_shelx_estimated_absorpt_T_max   0.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.24024
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            4025
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.428
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1092
_reflns_number_gt                985
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2018)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0288P)²] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1092
_refine_ls_number_parameters     65
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0571
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_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
Cu1 Cu 0.5000 0.5000 0.5000 0.03053(18) Uani 1 2 d S . P . .
O1 O 0.4170(2) 0.64673(19) 0.64922(16) 0.0252(4) Uani 1 1 d . . . . .
C1 C 0.3443(3) 0.7854(3) 0.5980(3) 0.0213(5) Uani 1 1 d . . . . .
C2 C 0.3024(4) 0.8125(3) 0.4366(2) 0.0244(5) Uani 1 1 d . . . . .
H2A H 0.1720 0.8583 0.4046 0.029 Uiso 1 1 calc R U . . .
H2B H 0.3945 0.8938 0.4113 0.029 Uiso 1 1 calc R U . . .
N2 N 0.3192(3) 0.6482(2) 0.3655(2) 0.0266(5) Uani 1 1 d . . . . .
H2D H 0.3638 0.6647 0.2846 0.032 Uiso 1 1 calc R U . . .
H2C H 0.2026 0.5987 0.3416 0.032 Uiso 1 1 calc R U . . .
N1 N 0.3084(3) 0.9103(2) 0.6811(2) 0.0305(5) Uani 1 1 d . . . . .
H1A H 0.3348 0.8985 0.7739 0.037 Uiso 1 1 calc R U . . .
H1B H 0.2583 1.0043 0.6428 0.037 Uiso 1 1 calc R U . . .
Cl Cl 0.182(2) 0.269(2) 0.475(2) 0.0288(3) Uani 0.351(3) 1 d . U P A 1
Br Br 0.1606(5) 0.2728(5) 0.4783(5) 0.0288(3) Uani 0.649(3) 1 d . U P A 2


_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
Cu1 N2 1.971(2) 3_666 ?
Cu1 N2 1.971(2) . ?
Cu1 O1 1.9907(14) . ?
Cu1 O1 1.9907(14) 3_666 ?
O1 C1 1.250(3) . ?
C1 N1 1.307(3) . ?
C1 C2 1.501(3) . ?
C2 N2 1.464(3) . ?

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
N2 Cu1 N2 180.0 3_666 . ?
N2 Cu1 O1 97.37(7) 3_666 . ?
N2 Cu1 O1 82.63(7) . . ?
N2 Cu1 O1 82.63(7) 3_666 3_666 ?
N2 Cu1 O1 97.37(7) . 3_666 ?
O1 Cu1 O1 180.00(7) . 3_666 ?
C1 O1 Cu1 112.47(14) . . ?
O1 C1 N1 122.0(2) . . ?
O1 C1 C2 119.42(19) . . ?
N1 C1 C2 118.5(2) . . ?
N2 C2 C1 108.76(17) . . ?
C2 N2 Cu1 108.86(14) . . ?

_refine_diff_density_max         0.295
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.086

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1915364'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'diaquabis(glycinamide)nickel(II) chloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 N4 Ni O4, Cl2'
_chemical_formula_sum            'C4 H16 Cl2 N4 Ni O4'
_chemical_formula_weight         313.82

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   11.2394(5)
_cell_length_b                   11.2394(5)
_cell_length_c                   37.594(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4749.0(6)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7062
_cell_measurement_theta_min      4.8270
_cell_measurement_theta_max      32.7600

_exptl_crystal_description       prism
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_F_000             2592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.086
_shelx_estimated_absorpt_T_min   0.368
_shelx_estimated_absorpt_T_max   0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            21338
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         4.369
_diffrn_reflns_theta_max         32.974
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4042
_reflns_number_gt                3480
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_max     0.934
_reflns_Friedel_fraction_full    0.993

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;

_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0251P)²+1.4396P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.473(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4042
_refine_ls_number_parameters     149
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0592
_refine_ls_wR_factor_gt          0.0550
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
O1W O 0.64566(17) 0.43846(14) 0.93069(7) 0.0307(4) Uani 1 1 d D . . . .
O11 O 0.4379(2) 0.3493(2) 0.96988(6) 0.0325(5) Uani 1 1 d . . . . .
O12 O 0.4362(2) 0.3588(2) 0.89257(6) 0.0319(5) Uani 1 1 d . . . . .
N22 N 0.6346(2) 0.2294(2) 0.88538(7) 0.0295(5) Uani 1 1 d . . . . .
H22C H 0.7024 0.2699 0.8839 0.035 Uiso 1 1 calc R U . . .
H22D H 0.6522 0.1524 0.8869 0.035 Uiso 1 1 calc R U . . .
N21 N 0.6396(2) 0.2221(2) 0.97322(7) 0.0280(5) Uani 1 1 d . . . . .
H21D H 0.6562 0.1452 0.9705 0.034 Uiso 1 1 calc R U . . .
H21C H 0.7080 0.2618 0.9744 0.034 Uiso 1 1 calc R U . . .
O2W O 0.43863(19) 0.1279(2) 0.92948(9) 0.0465(5) Uani 1 1 d D . . . .
C22 C 0.5635(3) 0.2507(3) 0.85363(9) 0.0320(6) Uani 1 1 d . . . . .
H22B H 0.5321 0.1757 0.8450 0.038 Uiso 1 1 calc R U . . .
H22A H 0.6136 0.2844 0.8352 0.038 Uiso 1 1 calc R U . . .
C12 C 0.4623(3) 0.3342(3) 0.86125(9) 0.0268(6) Uani 1 1 d . . . . .
C11 C 0.4731(3) 0.3256(3) 1.00032(9) 0.0270(6) Uani 1 1 d . . . . .
C21 C 0.5719(3) 0.2397(3) 1.00624(9) 0.0317(6) Uani 1 1 d . . . . .
H21A H 0.6244 0.2697 1.0247 0.038 Uiso 1 1 calc R U . . .
H21B H 0.5397 0.1642 1.0142 0.038 Uiso 1 1 calc R U . . .
N11 N 0.4214(3) 0.3722(3) 1.02857(8) 0.0397(7) Uani 1 1 d . . . . .
H11A H 0.3622 0.4199 1.0260 0.048 Uiso 1 1 calc R U . . .
H11B H 0.4469 0.3549 1.0495 0.048 Uiso 1 1 calc R U . . .
Cl2 Cl 0.31813(7) 0.05054(7) 0.85542(2) 0.03705(18) Uani 1 1 d . . . . .
Cl1 Cl 0.45110(7) 0.30351(7) 0.75282(2) 0.03488(17) Uani 1 1 d . . . . .
N12 N 0.4028(3) 0.3778(3) 0.83455(7) 0.0409(7) Uani 1 1 d . . . . .
H12A H 0.3438 0.4248 0.8383 0.049 Uiso 1 1 calc R U . . .
H12B H 0.4225 0.3595 0.8131 0.049 Uiso 1 1 calc R U . . .
Ni1 Ni 0.54178(2) 0.28188(3) 0.93023(2) 0.02425(8) Uani 1 1 d . . . . .
H1WB H 0.667(3) 0.471(3) 0.9497(6) 0.036 Uiso 1 1 d D U . . .
H2WB H 0.390(3) 0.106(3) 0.9449(7) 0.036 Uiso 1 1 d D U . . .
H1WA H 0.620(3) 0.487(3) 0.9153(6) 0.036 Uiso 1 1 d D U . . .
H2WA H 0.425(3) 0.093(3) 0.9102(5) 0.036 Uiso 1 1 d D 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
O1W Ni1 2.1120(17) . ?
O11 C11 1.240(4) . ?
O11 Ni1 2.040(2) . ?
O12 C12 1.244(4) . ?
O12 Ni1 2.039(2) . ?
N22 C22 1.456(4) . ?
N22 Ni1 2.068(3) . ?
N21 C21 1.469(4) . ?
N21 Ni1 2.067(3) . ?
O2W Ni1 2.0831(19) . ?
C22 C12 1.502(5) . ?
C12 N12 1.301(4) . ?
C11 N11 1.319(4) . ?
C11 C21 1.488(5) . ?

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
C11 O11 Ni1 114.3(2) . . ?
C12 O12 Ni1 115.2(2) . . ?
C22 N22 Ni1 110.1(2) . . ?
C21 N21 Ni1 110.0(2) . . ?
N22 C22 C12 111.2(3) . . ?
O12 C12 N12 121.7(3) . . ?
O12 C12 C22 119.8(3) . . ?
N12 C12 C22 118.5(3) . . ?
O11 C11 N11 121.1(3) . . ?
O11 C11 C21 121.0(3) . . ?
N11 C11 C21 117.8(3) . . ?
N21 C21 C11 110.3(3) . . ?
O12 Ni1 O11 90.96(7) . . ?
O12 Ni1 N21 171.89(9) . . ?
O11 Ni1 N21 81.59(10) . . ?
O12 Ni1 N22 81.29(9) . . ?
O11 Ni1 N22 172.06(9) . . ?
N21 Ni1 N22 106.04(8) . . ?
O12 Ni1 O2W 91.09(11) . . ?
O11 Ni1 O2W 89.99(11) . . ?
N21 Ni1 O2W 92.10(12) . . ?
N22 Ni1 O2W 91.88(11) . . ?
O12 Ni1 O1W 88.52(10) . . ?
O11 Ni1 O1W 90.04(10) . . ?
N21 Ni1 O1W 88.29(10) . . ?
N22 Ni1 O1W 88.04(10) . . ?
O2W Ni1 O1W 179.61(12) . . ?

_refine_diff_density_max         0.432
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1915371'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        dichloro(glycinamide)copper(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 Cl2 Cu1 N4 O2'
_chemical_formula_sum            'C4 H12 Cl2 Cu N4 O2'
_chemical_formula_weight         282.62

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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                   6.8813(2)
_cell_length_b                   7.7420(2)
_cell_length_c                   9.2635(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.779(3)
_cell_angle_gamma                90
_cell_volume                     483.12(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7621
_cell_measurement_theta_min      4.8620
_cell_measurement_theta_max      32.4060

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_F_000             286
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    2.787
_shelx_estimated_absorpt_T_min   0.367
_shelx_estimated_absorpt_T_max   0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            11873
_diffrn_reflns_av_unetI/netI     0.0071
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.284
_diffrn_reflns_theta_max         27.979
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1159
_reflns_number_gt                1139
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2014)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0365P)²+0.1145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.073(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1159
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0479
_refine_ls_wR_factor_gt          0.0477
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
Cu1 Cu 1.0000 0.0000 0.5000 0.02605(10) Uani 1 2 d S . P . .
Cl Cl 0.67343(4) -0.22657(4) 0.48141(3) 0.02892(11) Uani 1 1 d . . . . .
O1 O 1.08718(11) -0.14842(10) 0.34952(8) 0.02258(17) Uani 1 1 d . . . . .
N2 N 1.18488(15) -0.14907(12) 0.63818(10) 0.0244(2) Uani 1 1 d . . . . .
N1 N 1.19781(16) -0.41585(14) 0.31811(12) 0.0281(2) Uani 1 1 d . . . . .
C1 C 1.16050(14) -0.28856(13) 0.40173(11) 0.0188(2) Uani 1 1 d . . . . .
C2 C 1.20256(16) -0.31574(14) 0.56680(11) 0.0214(2) Uani 1 1 d . . . . .
H2B H 1.328(2) -0.368(2) 0.5968(18) 0.034(4) Uiso 1 1 d . . . . .
H2D H 1.307(3) -0.085(3) 0.656(2) 0.044(5) Uiso 1 1 d . . . . .
H2A H 1.102(2) -0.389(2) 0.5858(17) 0.028(3) Uiso 1 1 d . . . . .
H2C H 1.159(3) -0.164(3) 0.723(2) 0.048(5) Uiso 1 1 d . . . . .
H1A H 1.180(2) -0.396(2) 0.229(2) 0.040(4) Uiso 1 1 d . . . . .
H1B H 1.243(3) -0.505(2) 0.358(2) 0.035(5) Uiso 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
Cu1 N2 1.9809(9) 3_756 ?
Cu1 N2 1.9810(9) . ?
Cu1 O1 1.9912(7) . ?
Cu1 O1 1.9912(7) 3_756 ?
O1 C1 1.2515(13) . ?
N2 C2 1.4663(14) . ?
N2 H2D 0.96(2) . ?
N2 H2C 0.85(2) . ?
N1 C1 1.3109(14) . ?
N1 H1A 0.824(19) . ?
N1 H1B 0.817(18) . ?
C1 C2 1.5118(14) . ?
C2 H2B 0.944(16) . ?
C2 H2A 0.936(16) . ?

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
N2 Cu1 N2 180.0 3_756 . ?
N2 Cu1 O1 97.43(4) 3_756 . ?
N2 Cu1 O1 82.57(4) . . ?
N2 Cu1 O1 82.57(4) 3_756 3_756 ?
N2 Cu1 O1 97.43(4) . 3_756 ?
O1 Cu1 O1 180.00(3) . 3_756 ?
C1 O1 Cu1 112.65(6) . . ?
C2 N2 Cu1 108.83(7) . . ?
C2 N2 H2D 112.3(11) . . ?
Cu1 N2 H2D 103.7(11) . . ?
C2 N2 H2C 110.7(13) . . ?
Cu1 N2 H2C 116.4(13) . . ?
H2D N2 H2C 104.7(16) . . ?
C1 N1 H1A 116.5(13) . . ?
C1 N1 H1B 118.2(14) . . ?
H1A N1 H1B 125.1(19) . . ?
O1 C1 N1 122.38(10) . . ?
O1 C1 C2 119.37(9) . . ?
N1 C1 C2 118.23(10) . . ?
N2 C2 C1 108.50(8) . . ?
N2 C2 H2B 113.6(10) . . ?
C1 C2 H2B 109.4(10) . . ?
N2 C2 H2A 108.4(10) . . ?
C1 C2 H2A 106.2(9) . . ?
H2B C2 H2A 110.5(14) . . ?

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
Cu1 O1 C1 N1 168.85(8) . . . . ?
Cu1 O1 C1 C2 -9.27(11) . . . . ?
Cu1 N2 C2 C1 26.66(10) . . . . ?
O1 C1 C2 N2 -12.03(13) . . . . ?
N1 C1 C2 N2 169.78(10) . . . . ?

_refine_diff_density_max         0.422
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.048


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1915368'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'diaquabis(glycinamide)cobalt(II) chloride'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 Co N4 O4, Cl2'
_chemical_formula_sum            'C4 H16 Cl2 Co N4 O4'
_chemical_formula_weight         314.04

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_H-M_alt        'I 41 c d'
_space_group_name_Hall           'I 4bw -2c'

_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'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   11.3145(2)
_cell_length_b                   11.3145(2)
_cell_length_c                   37.9735(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4861.3(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13056
_cell_measurement_theta_min      4.8100
_cell_measurement_theta_max      32.5810

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_F_000             2576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.853
_shelx_estimated_absorpt_T_min   0.555
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66183
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            26763
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         4.193
_diffrn_reflns_theta_max         26.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2660
_reflns_number_gt                2592
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.995

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.0228P)²+1.1329P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.391(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2660
_refine_ls_number_parameters     153
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0169
_refine_ls_wR_factor_ref         0.0426
_refine_ls_wR_factor_gt          0.0423
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.128
_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
C12 C 0.3276(3) -0.0285(3) 0.84428(8) 0.0260(5) Uani 1 1 d . . . . .
C22 C 0.2425(3) 0.0715(3) 0.85048(9) 0.0307(6) Uani 1 1 d . . . . .
H22B H 0.1674 0.0401 0.8585 0.037 Uiso 1 1 calc R U . . .
H22A H 0.2733 0.1230 0.8687 0.037 Uiso 1 1 calc R U . . .
C11 C 0.3368(3) -0.0397(2) 0.70348(8) 0.0269(6) Uani 1 1 d . . . . .
C21 C 0.2545(3) 0.0614(2) 0.69539(9) 0.0317(6) Uani 1 1 d . . . . .
H21A H 0.2892 0.1106 0.6772 0.038 Uiso 1 1 calc R U . . .
H21B H 0.1804 0.0304 0.6865 0.038 Uiso 1 1 calc R U . . .
N12 N 0.3741(3) -0.0805(2) 0.87220(7) 0.0389(6) Uani 1 1 d . . . . .
H12A H 0.4210 -0.1397 0.8696 0.047 Uiso 1 1 calc R U . . .
H12B H 0.3574 -0.0552 0.8930 0.047 Uiso 1 1 calc R U . . .
N22 N 0.22441(19) 0.1399(2) 0.81796(7) 0.0275(5) Uani 1 1 d . . . . .
H22C H 0.2647 0.2073 0.8192 0.033 Uiso 1 1 calc R U . . .
H22D H 0.1481 0.1575 0.8157 0.033 Uiso 1 1 calc R U . . .
N11 N 0.3799(3) -0.0995(2) 0.67698(7) 0.0412(6) Uani 1 1 d . . . . .
H11A H 0.4262 -0.1584 0.6808 0.049 Uiso 1 1 calc R U . . .
H11B H 0.3618 -0.0800 0.6558 0.049 Uiso 1 1 calc R U . . .
N21 N 0.2316(2) 0.13330(19) 0.72670(7) 0.0287(5) Uani 1 1 d . . . . .
H21D H 0.1551 0.1511 0.7277 0.034 Uiso 1 1 calc R U . . .
H21C H 0.2721 0.2006 0.7252 0.034 Uiso 1 1 calc R U . . .
O12 O 0.35012(19) -0.06317(19) 0.81401(6) 0.0322(4) Uani 1 1 d . . . . .
O11 O 0.36081(18) -0.06513(18) 0.73474(6) 0.0316(4) Uani 1 1 d . . . . .
Co1 Co 0.28150(2) 0.04187(2) 0.77335(4) 0.02406(8) Uani 1 1 d . . . . .
O1W O 0.44043(12) 0.14513(14) 0.77388(4) 0.0308(3) Uani 1 1 d D . . . .
O2W O 0.12907(16) -0.06381(15) 0.77259(3) 0.0461(4) Uani 1 1 d D . . . .
H1WA H 0.4780(4) 0.1527(17) 0.79312(8) 0.087(15) Uiso 1 1 d D . . . .
H1WB H 0.4931(4) 0.1323(15) 0.75839(10) 0.048(10) Uiso 1 1 d D . . . .
H2WA H 0.0941(7) -0.1027(7) 0.78865(9) 0.071(14) Uiso 1 1 d D . . . .
H2WB H 0.0956(8) -0.0844(10) 0.75352(7) 0.093(17) Uiso 1 1 d D . . . .
Cl1 Cl 0.54984(6) -0.32052(6) 0.69888(5) 0.03598(16) Uani 1 1 d . . . . .
Cl2 Cl 0.54813(6) -0.30591(6) 0.84565(5) 0.03398(16) 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
C12 O12 1.241(3) . ?
C12 N12 1.322(4) . ?
C12 C22 1.504(4) . ?
C22 N22 1.472(4) . ?
C11 O11 1.251(3) . ?
C11 N11 1.307(4) . ?
C11 C21 1.506(4) . ?
C21 N21 1.464(4) . ?
N22 Co1 2.125(2) . ?
N21 Co1 2.128(2) . ?
O12 Co1 2.0973(19) . ?
O11 Co1 2.1027(19) . ?
Co1 O2W 2.0988(17) . ?
Co1 O1W 2.1445(15) . ?

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
O12 C12 N12 121.4(3) . . ?
O12 C12 C22 120.9(3) . . ?
N12 C12 C22 117.7(2) . . ?
N22 C22 C12 110.7(2) . . ?
O11 C11 N11 122.0(3) . . ?
O11 C11 C21 120.2(3) . . ?
N11 C11 C21 117.8(3) . . ?
N21 C21 C11 111.4(2) . . ?
C22 N22 Co1 110.59(17) . . ?
C21 N21 Co1 111.05(18) . . ?
C12 O12 Co1 115.27(19) . . ?
C11 O11 Co1 115.85(18) . . ?
O12 Co1 O2W 89.52(9) . . ?
O12 Co1 O11 91.67(6) . . ?
O2W Co1 O11 90.75(8) . . ?
O12 Co1 N22 79.73(8) . . ?
O2W Co1 N22 93.36(9) . . ?
O11 Co1 N22 170.42(8) . . ?
O12 Co1 N21 170.60(8) . . ?
O2W Co1 N21 92.73(9) . . ?
O11 Co1 N21 79.19(8) . . ?
N22 Co1 N21 109.22(7) . . ?
O12 Co1 O1W 89.51(8) . . ?
O2W Co1 O1W 178.26(7) . . ?
O11 Co1 O1W 87.84(8) . . ?
N22 Co1 O1W 87.88(8) . . ?
N21 Co1 O1W 88.00(8) . . ?

_refine_diff_density_max         0.156
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.036


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_2c_LT
_database_code_depnum_ccdc_archive 'CCDC 1915370'
loop_
_audit_author_name
_audit_author_address
'Darko Vusak'
;Department of Chemistry, Faculty of Science, University of Zagreb
Croatia
;
_audit_update_record             
;
2019-05-10 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        'diaquabis(glycinamide)nickel(II) iodide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H16 N4 Ni O4, I2'
_chemical_formula_sum            'C4 H16 I2 N4 Ni O4'
_chemical_formula_weight         496.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Ni Ni 0.3393 1.1124 '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           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   7.2589(7)
_cell_length_b                   10.3706(10)
_cell_length_c                   19.2258(17)
_cell_angle_alpha                90
_cell_angle_beta                 98.742(9)
_cell_angle_gamma                90
_cell_volume                     1430.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1109
_cell_measurement_theta_min      5.0510
_cell_measurement_theta_max      31.9250

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    5.675
_shelx_estimated_absorpt_T_min   0.199
_shelx_estimated_absorpt_T_max   0.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_reflns_number            2506
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.288
_diffrn_reflns_theta_max         26.989
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2506
_reflns_number_gt                2208
_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       'CrysAlis CCD (Oxford Diffraction,2010)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2018)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (C.F. Macrae et al , 2008)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0549P)²+2.1388P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2506
_refine_ls_number_parameters     78
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.1020
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_refine_ls_shift/su_max          0.000
_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
N1 N 0.1131(8) 1.0082(6) 0.3117(3) 0.0336(13) Uani 1 1 d . . . . .
H1A H 0.1134 1.0913 0.3210 0.040 Uiso 1 1 calc R U . . .
H1B H 0.0889 0.9811 0.2679 0.040 Uiso 1 1 calc R U . . .
C1 C 0.1488(8) 0.9243(6) 0.3634(3) 0.0213(13) Uani 1 1 d . . . . .
H1WA H 0.577(9) 0.887(3) 0.469(4) 0.03(2) Uiso 1 1 d D . . . .
H1WB H 0.571(12) 0.753(4) 0.464(5) 0.08(4) Uiso 1 1 d D . . . .
I1 I 0.15582(7) 0.36412(4) 0.34672(2) 0.02828(17) Uani 1 1 d . . . . .
Ni1 Ni 0.2500 0.81934(10) 0.5000 0.0217(3) Uani 1 2 d S T P . .
O1W O 0.5258(7) 0.8198(5) 0.4814(3) 0.0286(10) Uani 1 1 d D . . . .
O1 O 0.1842(6) 0.9622(4) 0.4274(2) 0.0249(9) Uani 1 1 d . . . . .
C2 C 0.1502(10) 0.7841(6) 0.3476(3) 0.0270(13) Uani 1 1 d . . . . .
H2A H 0.0354 0.7615 0.3152 0.032 Uiso 1 1 calc R U . . .
H2B H 0.2582 0.7643 0.3236 0.032 Uiso 1 1 calc R U . . .
N2 N 0.1613(8) 0.7048(5) 0.4122(3) 0.0272(12) Uani 1 1 d . . . . .
H2C H 0.2428 0.6387 0.4103 0.033 Uiso 1 1 calc R U . . .
H2D H 0.0473 0.6708 0.4154 0.033 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
N1 C1 1.316(8) . ?
C1 O1 1.281(7) . ?
C1 C2 1.485(9) . ?
Ni1 O1 2.041(4) . ?
Ni1 O1 2.041(4) 2_556 ?
Ni1 N2 2.084(5) . ?
Ni1 N2 2.084(5) 2_556 ?
Ni1 O1W 2.087(5) 2_556 ?
Ni1 O1W 2.087(5) . ?
C2 N2 1.482(8) . ?

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 C1 N1 120.7(6) . . ?
O1 C1 C2 119.4(5) . . ?
N1 C1 C2 119.9(6) . . ?
O1 Ni1 O1 86.9(2) . 2_556 ?
O1 Ni1 N2 81.29(19) . . ?
O1 Ni1 N2 168.08(18) 2_556 . ?
O1 Ni1 N2 168.08(19) . 2_556 ?
O1 Ni1 N2 81.29(19) 2_556 2_556 ?
N2 Ni1 N2 110.5(3) . 2_556 ?
O1 Ni1 O1W 89.14(19) . 2_556 ?
O1 Ni1 O1W 90.69(19) 2_556 2_556 ?
N2 Ni1 O1W 87.4(2) . 2_556 ?
N2 Ni1 O1W 92.8(2) 2_556 2_556 ?
O1 Ni1 O1W 90.69(19) . . ?
O1 Ni1 O1W 89.14(19) 2_556 . ?
N2 Ni1 O1W 92.8(2) . . ?
N2 Ni1 O1W 87.3(2) 2_556 . ?
O1W Ni1 O1W 179.8(3) 2_556 . ?
C1 O1 Ni1 115.2(4) . . ?
N2 C2 C1 111.9(5) . . ?
C2 N2 Ni1 109.5(4) . . ?

_refine_diff_density_max         2.278
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.185


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
