# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_NiMOF
_database_code_depnum_ccdc_archive 'CCDC 2020900'
loop_
_audit_author_name
_audit_author_address
'XinxinXu '
;Department of Chemistry
China
;
_audit_update_record             
;
2020-08-12 deposited with the CCDC.	2020-08-14 downloaded from the CCDC.
;
_audit_creation_date             2020-08-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C50 H48 N4 Ni4 O22 S4), 2(H2 O)'
_chemical_formula_sum            'C25 H28 N2 Ni2 O13 S2'
_chemical_formula_weight         746.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.3634(7)
_cell_length_b                   10.5517(3)
_cell_length_c                   16.4604(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.198(4)
_cell_angle_gamma                90
_cell_volume                     3212.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4130
_cell_measurement_theta_min      3.7010
_shelx_estimated_absorpt_T_max   0.54
_shelx_estimated_absorpt_T_min   0.21
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5888
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.629
_diffrn_reflns_theta_min         3.653
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5059
_reflns_number_total             5888
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.803
_refine_diff_density_min         -3.177
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0600
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²+25.1720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1774
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.685
 0.315
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O6-H6
 0.85 with sigma of 0.02
4. Rigid bond restraints
 O0AA, O1AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O0AA \\sim O1AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
6. Others
 Fixed Sof: H13A(0.5) H13B(0.5) O0AA(0.5) H0AA(0.5) H0AB(0.5) O1AA(0.5)
 H1AA(0.5) H1AB(0.5)
7.a Riding coordinates:
 O0AA(H0AA,H0AB), O1AA(H1AA,H1AB)
7.b Rotating group:
 O5(H5A,H5B)
7.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C7(H7), C11(H11), C3(H3), C8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.00550(2) 0.61980(4) 0.14252(3) 0.01374(12) Uani 1 1 d . . . . .
S1 S -0.23592(6) 0.82391(13) 0.23902(7) 0.0333(3) Uani 1 1 d . . . . .
O6 O 0.000000 0.5117(3) 0.250000 0.0168(6) Uani 1 2 d DS T P . .
O1 O -0.08134(15) 0.7199(3) 0.14896(18) 0.0264(6) Uani 1 1 d . . . . .
N1 N 0.00654(18) 0.7358(3) 0.04104(19) 0.0212(6) Uani 1 1 d . . . . .
O5 O -0.06571(17) 0.4940(3) 0.0609(2) 0.0303(6) Uani 1 1 d . . . . .
H5A H -0.110788 0.497693 0.066588 0.045 Uiso 1 1 d GR . . . .
H5B H -0.054064 0.411577 0.073702 0.045 Uiso 1 1 d GR . . . .
O3 O -0.37734(19) 0.9164(4) 0.2484(2) 0.0422(9) Uani 1 1 d . . . . .
C5 C -0.10984(17) 0.7467(3) 0.2057(2) 0.0174(6) Uani 1 1 d . . . . .
C4 C -0.2988(2) 0.9094(4) 0.1642(3) 0.0262(8) Uani 1 1 d . . . . .
C2 C -0.2095(3) 0.8738(6) 0.1007(3) 0.0441(14) Uani 1 1 d . . . . .
H2 H -0.187693 0.876311 0.057463 0.053 Uiso 1 1 calc R . . . .
C13 C 0.000000 0.8923(6) -0.250000 0.0400(17) Uani 1 2 d S T P . .
H13A H -0.042376 0.838250 -0.262815 0.048 Uiso 0.5 1 calc R . . . .
H13B H 0.042374 0.838244 -0.237186 0.048 Uiso 0.5 1 calc R . . . .
C1 C -0.18028(19) 0.8143(4) 0.1760(2) 0.0231(7) Uani 1 1 d . . . . .
C10 C 0.0685(3) 0.8606(5) -0.0362(3) 0.0404(11) Uani 1 1 d . . . . .
H10 H 0.112273 0.890925 -0.041031 0.049 Uiso 1 1 calc R . . . .
C9 C 0.0041(3) 0.8934(4) -0.0963(3) 0.0353(10) Uani 1 1 d . . . . .
C7 C -0.0557(2) 0.7679(4) -0.0166(3) 0.0284(8) Uani 1 1 d . . . . .
H7 H -0.098771 0.736610 -0.010335 0.034 Uiso 1 1 calc R . . . .
C11 C 0.0673(2) 0.7822(4) 0.0311(3) 0.0306(8) Uani 1 1 d . . . . .
H11 H 0.110904 0.761294 0.070979 0.037 Uiso 1 1 calc R . . . .
C18 C 0.0027(4) 0.9733(5) -0.1726(3) 0.0470(14) Uani 1 1 d . . . . .
H18A H 0.045599 1.026202 -0.159222 0.056 Uiso 1 1 calc R . . . .
H18B H -0.039163 1.028465 -0.185837 0.056 Uiso 1 1 calc R . . . .
C3 C -0.2761(2) 0.9312(6) 0.0947(3) 0.0436(13) Uani 1 1 d . . . . .
H3 H -0.302057 0.979098 0.048285 0.052 Uiso 1 1 calc R . . . .
C8 C -0.0586(3) 0.8454(5) -0.0850(3) 0.0378(10) Uani 1 1 d . . . . .
H8 H -0.103016 0.865364 -0.123577 0.045 Uiso 1 1 calc R . . . .
O2 O -0.08646(15) 0.7251(3) 0.28321(17) 0.0261(6) Uani 1 1 d . . . . .
C6 C -0.3677(2) 0.9482(4) 0.1793(3) 0.0262(8) Uani 1 1 d . . . . .
O4 O -0.41231(15) 1.0097(3) 0.12066(18) 0.0259(6) Uani 1 1 d . . . . .
H6 H -0.040(2) 0.473(6) 0.246(4) 0.054(19) Uiso 1 1 d D . . . .
O0AA O -0.1893(13) 0.361(2) 0.0805(12) 0.131(9) Uani 0.5 1 d . U . A 1
H0AA H -0.224458 0.318362 0.049635 0.196 Uiso 0.5 1 d R . . A 1
H0AB H -0.165318 0.308712 0.117285 0.196 Uiso 0.5 1 d R . . A 1
O1AA O -0.2023(10) 0.467(3) 0.0924(10) 0.143(10) Uani 0.5 1 d . U . B 2
H1AA H -0.201483 0.430012 0.138465 0.214 Uiso 0.5 1 d R . . B 2
H1AB H -0.242403 0.506322 0.077785 0.214 Uiso 0.5 1 d R . . 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 O6 2.1337(19) . ?
Ni1 O1 2.015(3) . ?
Ni1 N1 2.076(3) . ?
Ni1 O5 2.091(3) . ?
Ni1 O2 2.013(3) 2 ?
Ni1 O4 2.086(3) 3_545 ?
S1 C4 1.710(4) . ?
S1 C1 1.705(4) . ?
O1 C5 1.250(4) . ?
N1 C7 1.339(5) . ?
N1 C11 1.328(5) . ?
O3 C6 1.251(5) . ?
C5 C1 1.488(5) . ?
C5 O2 1.242(4) . ?
C4 C3 1.360(6) . ?
C4 C6 1.485(5) . ?
C2 C1 1.356(6) . ?
C2 C3 1.402(6) . ?
C13 C18 1.521(6) . ?
C13 C18 1.521(6) 2_554 ?
C10 C9 1.388(8) . ?
C10 C11 1.389(6) . ?
C9 C18 1.507(6) . ?
C9 C8 1.378(8) . ?
C7 C8 1.379(6) . ?
C6 O4 1.267(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 O6 89.39(10) . . ?
O1 Ni1 N1 86.56(12) . . ?
O1 Ni1 O5 87.95(13) . . ?
O1 Ni1 O4 172.86(12) . 3_545 ?
N1 Ni1 O6 175.61(11) . . ?
N1 Ni1 O5 91.08(13) . . ?
N1 Ni1 O4 90.01(12) . 3_545 ?
O5 Ni1 O6 90.48(11) . . ?
O2 Ni1 O6 90.70(10) 2 . ?
O2 Ni1 O1 101.01(13) 2 . ?
O2 Ni1 N1 88.40(12) 2 . ?
O2 Ni1 O5 170.97(13) 2 . ?
O2 Ni1 O4 85.14(13) 2 3_545 ?
O4 Ni1 O6 94.19(10) 3_545 . ?
O4 Ni1 O5 85.84(13) 3_545 . ?
C1 S1 C4 92.12(19) . . ?
Ni1 O6 Ni1 115.39(16) . 2 ?
C5 O1 Ni1 135.9(2) . . ?
C7 N1 Ni1 119.9(3) . . ?
C11 N1 Ni1 122.4(3) . . ?
C11 N1 C7 117.7(4) . . ?
O1 C5 C1 115.3(3) . . ?
O2 C5 O1 128.2(3) . . ?
O2 C5 C1 116.5(3) . . ?
C3 C4 S1 110.9(3) . . ?
C3 C4 C6 128.5(4) . . ?
C6 C4 S1 120.6(3) . . ?
C1 C2 C3 113.1(4) . . ?
C18 C13 C18 111.7(5) . 2_554 ?
C5 C1 S1 120.8(3) . . ?
C2 C1 S1 111.1(3) . . ?
C2 C1 C5 128.1(3) . . ?
C9 C10 C11 119.5(5) . . ?
C10 C9 C18 121.6(5) . . ?
C8 C9 C10 117.0(4) . . ?
C8 C9 C18 121.3(5) . . ?
N1 C7 C8 122.6(4) . . ?
N1 C11 C10 122.9(4) . . ?
C9 C18 C13 111.8(4) . . ?
C4 C3 C2 112.7(4) . . ?
C9 C8 C7 120.3(5) . . ?
C5 O2 Ni1 135.0(2) . 2 ?
O3 C6 C4 117.5(3) . . ?
O3 C6 O4 125.3(4) . . ?
O4 C6 C4 117.3(4) . . ?
C6 O4 Ni1 122.5(2) . 3_455 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.685
2 0.315

