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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc1zmj15
_database_code_depnum_ccdc_archive 'CCDC 1836007'
_audit_update_record             
;
2018-04-10 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ([MnNi(CN)4(H2O)2].3H2)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H10 Mn N4 Ni O6'
_chemical_formula_weight         323.81

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'
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'
Mn Mn 0.3368 0.7283 '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'
H H 0.0000 0.0000 '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                   12.0750(3)
_cell_length_b                   14.0779(3)
_cell_length_c                   7.3144(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1243.38(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_F_000             652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    2.546
_shelx_estimated_absorpt_T_min   0.646
_shelx_estimated_absorpt_T_max   0.743
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33643
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.894
_diffrn_reflns_theta_max         46.312
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5544
_reflns_number_gt                5023
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0400P)²+0.1793P] 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         5544
_refine_ls_number_parameters     107
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.102
_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
Ni Ni 0.57158(2) 0.250000 0.48839(2) 0.00740(2) Uani 1 2 d S T P . .
Mn Mn 0.500000 0.500000 1.000000 0.00723(2) Uani 1 2 d S . P . .
O1 O 0.32152(4) 0.43146(3) 0.45703(7) 0.01589(7) Uani 1 1 d D . . . .
H1A H 0.3771(16) 0.4450(15) 0.5101(19) 0.041(5) Uiso 1 1 d . . . . .
H1B H 0.335(4) 0.433(3) 0.342(3) 0.234(19) Uiso 1 1 d D . . . .
O2 O 0.24781(6) 0.250000 0.55978(10) 0.01778(10) Uani 1 2 d DS T P . .
H2A H 0.173(3) 0.250000 0.518(3) 0.058(9) Uiso 1 2 d S . P . .
H2B H 0.3101(19) 0.250000 0.540(9) 0.28(5) Uiso 1 2 d DS . P . .
O3 O 0.28757(6) 0.250000 0.94418(10) 0.01772(10) Uani 1 2 d S T P . .
H3A H 0.308(3) 0.288(2) 0.992(3) 0.021(7) Uiso 0.5 1 d . . P . .
H3B H 0.282(2) 0.250000 0.842(4) 0.057(7) Uiso 1 2 d S . P . .
O4 O 0.66422(3) 0.56377(3) 0.92892(6) 0.01321(6) Uani 1 1 d . . . . .
H4 H 0.7149(13) 0.5298(12) 0.959(2) 0.033(4) Uiso 1 1 d . . . . .
N1 N 0.52619(5) 0.39916(3) 0.77499(6) 0.01492(7) Uani 1 1 d . . . . .
N2 N 0.57463(4) 0.09916(3) 0.19538(7) 0.01356(7) Uani 1 1 d . . . . .
C1 C 0.54588(4) 0.34249(3) 0.66463(6) 0.01072(7) Uani 1 1 d . . . . .
C2 C 0.57765(4) 0.15705(4) 0.30821(7) 0.01035(7) 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
Ni C1 1.8583(5) . ?
Ni C1 1.8583(5) 7_565 ?
Ni C2 1.8587(5) 7_565 ?
Ni C2 1.8587(5) . ?
Mn N2 2.1916(4) 7_566 ?
Mn N2 2.1916(4) 3_656 ?
Mn N1 2.1963(4) 5_667 ?
Mn N1 2.1963(4) . ?
Mn O4 2.2380(4) 5_667 ?
Mn O4 2.2380(4) . ?
N1 C1 1.1596(6) . ?
N2 C2 1.1604(7) . ?

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
C1 Ni C1 88.96(3) . 7_565 ?
C1 Ni C2 90.30(2) . 7_565 ?
C1 Ni C2 172.63(2) 7_565 7_565 ?
C1 Ni C2 172.63(2) . . ?
C1 Ni C2 90.30(2) 7_565 . ?
C2 Ni C2 89.50(3) 7_565 . ?
N2 Mn N2 180.0 7_566 3_656 ?
N2 Mn N1 88.985(19) 7_566 5_667 ?
N2 Mn N1 91.015(19) 3_656 5_667 ?
N2 Mn N1 91.016(19) 7_566 . ?
N2 Mn N1 88.984(19) 3_656 . ?
N1 Mn N1 180.0 5_667 . ?
N2 Mn O4 87.554(17) 7_566 5_667 ?
N2 Mn O4 92.446(17) 3_656 5_667 ?
N1 Mn O4 87.571(18) 5_667 5_667 ?
N1 Mn O4 92.429(18) . 5_667 ?
N2 Mn O4 92.445(17) 7_566 . ?
N2 Mn O4 87.555(17) 3_656 . ?
N1 Mn O4 92.429(18) 5_667 . ?
N1 Mn O4 87.572(18) . . ?
O4 Mn O4 180.0 5_667 . ?
C1 N1 Mn 174.78(5) . . ?
C2 N2 Mn 157.52(4) . 3_646 ?
N1 C1 Ni 177.70(5) . . ?
N2 C2 Ni 175.93(5) . . ?

_refine_diff_density_max         3.337
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.194


_exptl_crystal_recrystallization_method ' slow diffusion method'
####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1855079'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_Int_Tables_number      62
_space_group_name_Hall           '-P 2ac 2n'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 -x,1/2+y,-z
4 1/2+x,1/2-y,1/2-z
5 -x,-y,-z
6 1/2+x,y,1/2-z
7 x,1/2-y,z
8 1/2-x,1/2+y,1/2+z
_cell_length_a                   12.3058(3)
_cell_length_b                   14.1261(3)
_cell_length_c                   7.3105(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1270.81
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ni Ni 0.43333(2) 0.250000 0.51028(2)
Mn Mn 0.500000 0.500000 1.000000
O O 0.66213(7) 0.43758(6) 0.93297(13)
H H 0.7012(18) 0.4603(18) 0.974(2)
N1 N 0.42973(8) 0.40066(7) 0.80111(12)
N2 N 0.47331(9) 0.10148(7) 0.22290(12)
C2 C 0.45572(8) 0.15781(6) 0.33311(11)
C1 C 0.42682(7) 0.34279(6) 0.68979(11)
O O 0.33787(7) 0.56242(6) 1.06703(13)
H H 0.2988(18) 0.5397(18) 1.026(2)
N1 N 0.57027(8) 0.59934(7) 1.19889(12)
C1 C 0.57318(7) 0.65721(6) 1.31021(11)
N2 N 0.47331(9) 0.39852(7) 0.22290(12)
C2 C 0.45572(8) 0.34219(6) 0.33311(11)
Ni Ni 0.56667(2) 0.750000 1.48972(2)
Mn Mn 0.500000 0.500000 0.000000
Mn Mn 0.500000 0.000000 0.000000
N2 N 0.52669(9) 0.60148(7) 0.77710(12)
N2 N 0.47331(9) 0.39852(7) 1.22290(12)
C1 C 0.42682(7) 0.15721(6) 0.68979(11)
OW1 O 0.21102(14) 0.250000 0.4409(2)
OW2 O 0.32059(9) 0.56711(9) 0.45547(18)
H2A H 0.361(2) 0.565(2) 0.490(3)
OW3 O 0.25259(17) 0.250000 0.0551(3)
H3A H 0.242(4) 0.213(5) -0.005(5)
H3B H 0.335(4) 0.277(3) 0.041(5)
H3A H 0.242(4) 0.287(5) -0.005(5)
H3B H 0.335(4) 0.223(3) 0.041(5)
