#------------------------------------------------------------------------------
#$Date: 2023-12-01 18:11:06 +0200 (Fri, 01 Dec 2023) $
#$Revision: 287938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/88/4508847.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4508847
loop_
_publ_author_name
'Zang, Shuangquan'
'Su, Yang'
'Song, You'
'Li, Yizhi'
'Ni, Zhaoping'
'Zhu, Huizhen'
'Meng, Qingjin'
_publ_section_title
;
 Tuning the Framework Formation of Ni(II) Complexes by Controlling the
 Hydrolysis of 2,2‘,3,3‘-Thiodiphthalic Dianhydride: 
 Syntheses, Crystal Structures, and Physical Properties
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2369
_journal_paper_doi               10.1021/cg060343u
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety
' 2(C36 H26 N4 Ni2 O10 S), 3.4(H4 O2), 4(H0.80 O0.40), H4 O2, H4 O2'
_chemical_formula_sum            'C72 H72 N8 Ni4 O30 S2'
_chemical_formula_weight         1828.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.145(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   25.122(7)
_cell_length_b                   8.253(2)
_cell_length_c                   11.259(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2218.3(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5992
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0700P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                3434
_reflns_number_total             4094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060343usup3.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     'C 2y '
_cod_original_sg_symbol_H-M      'C2 '
_cod_database_code               4508847
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.31378(2) 0.54981(6) 0.07006(5) 0.02932(16) Uani 1 1 d .
C3 C 0.35173(19) 0.1877(6) -0.0604(4) 0.0297(10) Uani 1 1 d .
C2 C 0.40087(19) 0.2772(6) -0.0010(4) 0.0286(10) Uani 1 1 d .
C1 C 0.4427(2) 0.2852(6) -0.0599(5) 0.0314(10) Uani 1 1 d .
C6 C 0.4368(2) 0.1978(7) -0.1699(5) 0.0441(13) Uani 1 1 d .
H6 H 0.4647 0.2023 -0.2082 0.053 Uiso 1 1 calc R
C5 C 0.3907(2) 0.1073(6) -0.2199(4) 0.0336(11) Uani 1 1 d .
H5 H 0.3870 0.0498 -0.2931 0.040 Uiso 1 1 calc R
C4 C 0.3486(2) 0.0979(6) -0.1644(5) 0.0349(11) Uani 1 1 d .
H4 H 0.3181 0.0300 -0.1981 0.042 Uiso 1 1 calc R
C7 C 0.30331(19) 0.1867(6) -0.0078(4) 0.0272(10) Uani 1 1 d .
C8 C 0.4116(2) 0.3600(6) 0.1250(5) 0.0329(11) Uani 1 1 d .
C9 C 0.2667(2) 0.5035(6) -0.2118(5) 0.0380(12) Uani 1 1 d .
H9 H 0.2356 0.4630 -0.1932 0.046 Uiso 1 1 calc R
C10 C 0.2672(2) 0.4974(6) -0.3321(5) 0.0358(12) Uani 1 1 d .
H10 H 0.2364 0.4567 -0.3943 0.043 Uiso 1 1 calc R
C11 C 0.31379(18) 0.5518(9) -0.3625(4) 0.0355(10) Uani 1 1 d .
C12 C 0.3580(2) 0.6177(7) -0.2659(5) 0.0389(12) Uani 1 1 d .
H12 H 0.3896 0.6584 -0.2822 0.047 Uiso 1 1 calc R
C13 C 0.3542(2) 0.6217(6) -0.1463(4) 0.0300(10) Uani 1 1 d .
H13 H 0.3839 0.6646 -0.0824 0.036 Uiso 1 1 calc R
C14 C 0.3465(2) 0.6484(7) 0.3398(4) 0.0381(12) Uani 1 1 d .
H14 H 0.3673 0.7248 0.3125 0.046 Uiso 1 1 calc R
C15 C 0.3460(2) 0.6570(7) 0.4650(5) 0.0392(12) Uani 1 1 d .
H15 H 0.3648 0.7394 0.5178 0.047 Uiso 1 1 calc R
C16 C 0.3165(2) 0.5382(8) 0.5073(4) 0.0380(11) Uani 1 1 d .
C17 C 0.2887(2) 0.4263(7) 0.4261(5) 0.0410(12) Uani 1 1 d .
H17 H 0.2678 0.3479 0.4510 0.049 Uiso 1 1 calc R
C18 C 0.2911(2) 0.4267(6) 0.3041(4) 0.0350(11) Uani 1 1 d .
H18 H 0.2723 0.3457 0.2497 0.042 Uiso 1 1 calc R
N1 N 0.30928(17) 0.5659(6) -0.1186(3) 0.0330(8) Uani 1 1 d .
N2 N 0.31942(15) 0.5397(7) 0.2616(3) 0.0341(8) Uani 1 1 d .
O3 O 0.29581(15) 0.3036(4) 0.0536(3) 0.0330(8) Uani 1 1 d .
O4 O 0.27123(12) 0.0693(4) -0.0377(3) 0.0288(6) Uani 1 1 d .
O1 O 0.39911(14) 0.5057(4) 0.1285(3) 0.0310(8) Uani 1 1 d .
O2 O 0.43433(15) 0.2733(4) 0.2173(4) 0.0396(9) Uani 1 1 d .
O5 O 0.32848(15) 0.7950(4) 0.0845(3) 0.0322(8) Uani 1 1 d .
H5C H 0.3288 0.8321 0.0143 0.039 Uiso 1 1 d R
H5A H 0.3587 0.8127 0.1376 0.039 Uiso 1 1 d R
O6 O 0.4311(3) 0.9429(7) 0.1875(6) 0.0432(15) Uani 0.60 1 d P
H6D H 0.4309 1.0064 0.2468 0.052 Uiso 0.60 1 d PR
H6C H 0.4467 0.9897 0.1397 0.052 Uiso 0.60 1 d PR
O7 O 0.5000 0.8491(8) 1.0000 0.0437(16) Uani 0.80 2 d SP
H7D H 0.4818 0.8734 1.0496 0.052 Uiso 0.40 1 d PR
H7B H 0.4780 0.8064 0.9342 0.052 Uiso 0.40 1 d PR
O8 O 0.4306(3) 0.2446(9) 0.4689(7) 0.0466(19) Uani 0.50 1 d P
H8B H 0.4041 0.2437 0.5010 0.056 Uiso 0.50 1 d PR
H8C H 0.4256 0.1691 0.4152 0.056 Uiso 0.50 1 d PR
O9 O 0.4466(3) 0.9515(9) 0.5317(7) 0.0390(16) Uani 0.50 1 d P
H9B H 0.4181 1.0113 0.5008 0.047 Uiso 0.50 1 d PR
H9C H 0.4725 0.9832 0.5034 0.047 Uiso 0.50 1 d PR
O10 O 0.5096(3) 0.5741(11) 0.3544(6) 0.0437(19) Uani 0.50 1 d P
H10D H 0.4919 0.6567 0.3170 0.052 Uiso 0.50 1 d PR
H10A H 0.5353 0.6042 0.4197 0.052 Uiso 0.50 1 d PR
S1 S 0.5000 0.4199(2) 0.0000 0.0284(3) Uani 1 2 d S
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'
S S 0.1246 0.1234 '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'
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
O5 Ni1 O4 95.05(14) . 4
O5 Ni1 O1 90.29(13) . .
O4 Ni1 O1 170.14(13) 4 .
O5 Ni1 O3 177.92(16) . .
O4 Ni1 O3 82.89(14) 4 .
O1 Ni1 O3 91.79(13) . .
O5 Ni1 N1 88.26(17) . .
O4 Ni1 N1 95.18(14) 4 .
O1 Ni1 N1 93.25(15) . .
O3 Ni1 N1 91.69(17) . .
O5 Ni1 N2 90.26(18) . .
O4 Ni1 N2 85.41(13) 4 .
O1 Ni1 N2 86.29(14) . .
O3 Ni1 N2 89.80(17) . .
N1 Ni1 N2 178.5(2) . .
C4 C3 C2 119.8(4) . .
C4 C3 C7 119.7(4) . .
C2 C3 C7 120.5(4) . .
C1 C2 C3 118.1(4) . .
C1 C2 C8 118.4(4) . .
C3 C2 C8 123.4(4) . .
C6 C1 C2 120.3(5) . .
C6 C1 S1 120.5(4) . .
C2 C1 S1 119.1(4) . .
C5 C6 C1 119.7(5) . .
C5 C6 H6 120.2 . .
C1 C6 H6 120.2 . .
C6 C5 C4 121.3(5) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
C3 C4 C5 120.5(5) . .
C3 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
O3 C7 O4 124.3(4) . .
O3 C7 C3 119.8(4) . .
O4 C7 C3 115.7(4) . .
O2 C8 O1 125.7(5) . .
O2 C8 C2 115.0(4) . .
O1 C8 C2 119.3(4) . .
N1 C9 C10 122.5(5) . .
N1 C9 H9 118.7 . .
C10 C9 H9 118.7 . .
C9 C10 C11 120.2(5) . .
C9 C10 H10 119.9 . .
C11 C10 H10 119.9 . .
C10 C11 C12 117.3(4) . .
C10 C11 C16 121.0(4) . 1_554
C12 C11 C16 121.6(4) . 1_554
C13 C12 C11 119.2(5) . .
C13 C12 H12 120.4 . .
C11 C12 H12 120.4 . .
N1 C13 C12 122.5(5) . .
N1 C13 H13 118.8 . .
C12 C13 H13 118.8 . .
N2 C14 C15 123.2(5) . .
N2 C14 H14 118.4 . .
C15 C14 H14 118.4 . .
C16 C15 C14 118.3(5) . .
C16 C15 H15 120.9 . .
C14 C15 H15 120.9 . .
C17 C16 C15 118.1(5) . .
C17 C16 C11 123.5(5) . 1_556
C15 C16 C11 118.2(4) . 1_556
C16 C17 C18 120.1(5) . .
C16 C17 H17 119.9 . .
C18 C17 H17 119.9 . .
N2 C18 C17 122.7(5) . .
N2 C18 H18 118.7 . .
C17 C18 H18 118.7 . .
C13 N1 C9 118.2(4) . .
C13 N1 Ni1 118.2(3) . .
C9 N1 Ni1 123.0(3) . .
C14 N2 C18 117.5(4) . .
C14 N2 Ni1 121.4(4) . .
C18 N2 Ni1 120.9(3) . .
C7 O3 Ni1 138.4(3) . .
C7 O4 Ni1 131.4(3) . 4_545
C8 O1 Ni1 114.0(3) . .
Ni1 O5 H5C 109.6 . .
Ni1 O5 H5A 109.6 . .
H5C O5 H5A 109.8 . .
H6D O6 H6C 109.5 . .
H7D O7 H7B 109.5 . .
H8B O8 H8C 109.5 . .
H9B O9 H9C 108.2 . .
H10D O10 H10A 109.5 . .
C1 S1 C1 102.6(3) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O5 2.055(3) .
Ni1 O4 2.058(3) 4
Ni1 O1 2.069(3) .
Ni1 O3 2.077(4) .
Ni1 N1 2.096(4) .
Ni1 N2 2.118(4) .
C3 C4 1.367(7) .
C3 C2 1.415(7) .
C3 C7 1.510(6) .
C2 C1 1.407(6) .
C2 C8 1.522(7) .
C1 C6 1.401(8) .
C1 S1 1.778(5) .
C6 C5 1.345(8) .
C6 H6 0.9300 .
C5 C4 1.388(7) .
C5 H5 0.9300 .
C4 H4 0.9300 .
C7 O3 1.235(6) .
C7 O4 1.238(6) .
C8 O2 1.244(6) .
C8 O1 1.247(6) .
C9 N1 1.346(7) .
C9 C10 1.360(7) .
C9 H9 0.9300 .
C10 C11 1.391(7) .
C10 H10 0.9300 .
C11 C12 1.400(7) .
C11 C16 1.493(6) 1_554
C12 C13 1.379(7) .
C12 H12 0.9300 .
C13 N1 1.343(6) .
C13 H13 0.9300 .
C14 N2 1.292(7) .
C14 C15 1.416(7) .
C14 H14 0.9300 .
C15 C16 1.399(8) .
C15 H15 0.9300 .
C16 C17 1.333(8) .
C16 C11 1.493(6) 1_556
C17 C18 1.393(7) .
C17 H17 0.9300 .
C18 N2 1.349(7) .
C18 H18 0.9300 .
O4 Ni1 2.058(3) 4_545
O5 H5C 0.8500 .
O5 H5A 0.8199 .
O6 H6D 0.8500 .
O6 H6C 0.8500 .
O7 H7D 0.8501 .
O7 H7B 0.8500 .
O8 H8B 0.8497 .
O8 H8C 0.8501 .
O9 H9B 0.8498 .
O9 H9C 0.8504 .
O10 H10D 0.8499 .
O10 H10A 0.8500 .
S1 C1 1.778(5) 2_655
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O6 0.82 2.04 2.761(7) 147.2 .
O8 H8C O2 0.85 2.46 2.874(9) 110.7 .
O6 H6D O2 0.85 2.23 2.746(7) 118.8 1_565
O9 H9B O8 0.85 2.00 2.517(10) 118.3 1_565
O7 H7D O6 0.85 2.36 3.213(7) 179.6 1_556
O9 H9C O9 0.85 2.20 2.985(15) 152.5 2_656
