#------------------------------------------------------------------------------
#$Date: 2019-11-17 07:41:45 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228714 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/83/1548396.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1548396
loop_
_publ_author_name
'Feng, Rui'
'Jia, Yan-Yuan'
'Li, Zhao-Yang'
'Chang, Ze'
'Bu, Xian-He'
_publ_section_title
;
 Enhancing the stability and porosity of penetrated metal-organic
 frameworks through the insertion of coordination sites.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              950
_journal_page_last               955
_journal_paper_doi               10.1039/c7sc04192f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C28 H30 N4 Ni2 O15 S'
_chemical_formula_weight         812.00
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
_symmetry_space_group_name_H-M   'I a -3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            48
_cell_length_a                   39.7584(2)
_cell_length_b                   39.7584(2)
_cell_length_c                   39.7584(2)
_cell_measurement_reflns_used    5610
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.2920
_cell_measurement_theta_min      4.1440
_cell_volume                     62847.3(5)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28035
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.453
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    1.702
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       block
_exptl_crystal_F_000             20064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF, CH3CN and H2O'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         2.091
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         10767
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1457P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7607
_reflns_number_total             10767
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7sc04192f2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1548396--1548397.cif.'
_cod_original_cell_volume        62847.3(9)
_cod_database_code               1548396
_shelx_shelxl_version_number     2016/6
_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+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
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
Ni1 Ni 0.78647(2) 0.73461(2) 0.88544(2) 0.01823(15) Uani 1 1 d . .
Ni2 Ni 0.82538(2) 0.74291(2) 0.96363(2) 0.02544(16) Uani 1 1 d . .
S1 S 0.51299(3) 0.69224(5) 0.99762(3) 0.0716(5) Uani 1 1 d . .
O13 O 0.79210(7) 0.71853(6) 0.93452(6) 0.0254(5) Uani 1 1 d D .
O1 O 0.73500(6) 0.72413(7) 0.88758(6) 0.0311(5) Uani 1 1 d . .
O3 O 0.77876(7) 0.75227(7) 0.83700(6) 0.0354(6) Uani 1 1 d . .
H3A H 0.787407 0.770496 0.828578 0.053 Uiso 1 1 d R U
H3B H 0.766356 0.742608 0.821814 0.053 Uiso 1 1 d R U
O9 O 0.84422(9) 0.69712(7) 0.98095(7) 0.0463(7) Uani 1 1 d . .
O2 O 0.72859(8) 0.72155(17) 0.94312(8) 0.093(2) Uani 1 1 d . .
C17 C 0.71731(9) 0.72071(14) 0.91350(10) 0.0443(11) Uani 1 1 d . .
C19 C 0.65937(10) 0.71236(13) 0.93658(9) 0.0449(11) Uani 1 1 d . .
H19 H 0.668351 0.714804 0.958038 0.054 Uiso 1 1 calc R U
O8 O 0.79107(9) 0.75008(12) 1.00021(8) 0.0634(10) Uani 1 1 d . .
H8A H 0.775386 0.762669 0.992706 0.095 Uiso 1 1 d R U
H8B H 0.800414 0.759619 1.016961 0.095 Uiso 1 1 d R U
N4 N 0.60489(8) 0.70561(13) 0.96220(8) 0.0506(11) Uani 1 1 d . .
H4 H 0.614254 0.711657 0.980740 0.061 Uiso 1 1 calc R U
C23 C 0.68035(9) 0.71502(12) 0.90856(9) 0.0364(9) Uani 1 1 d . .
C27 C 0.54089(10) 0.71189(15) 1.05174(10) 0.0505(12) Uani 1 1 d . .
H27 H 0.544370 0.717435 1.074197 0.061 Uiso 1 1 calc R U
C28 C 0.66674(8) 0.71147(11) 0.87655(8) 0.0323(8) Uani 1 1 d . .
H28 H 0.680352 0.713807 0.857668 0.039 Uiso 1 1 calc R U
C31 C 0.55539(10) 0.70152(17) 0.99673(10) 0.0545(14) Uani 1 1 d . .
C32 C 0.56705(11) 0.71222(15) 1.02741(10) 0.0524(12) Uani 1 1 d . .
H32 H 0.589093 0.718784 1.031691 0.063 Uiso 1 1 calc R U
O27 O 0.55545(9) 0.68661(18) 0.93972(9) 0.107(2) Uani 1 1 d . .
C34 C 0.62516(9) 0.70607(14) 0.93274(10) 0.0438(10) Uani 1 1 d . .
C37 C 0.57206(11) 0.69643(18) 0.96357(11) 0.0625(17) Uani 1 1 d . .
C39 C 0.51080(10) 0.70292(15) 1.03958(9) 0.0478(11) Uani 1 1 d . .
C42 C 0.61185(9) 0.70203(14) 0.90089(9) 0.0450(11) Uani 1 1 d . .
H42 H 0.589029 0.697705 0.898123 0.054 Uiso 1 1 calc R U
C45 C 0.61644(10) 0.70157(13) 0.83873(9) 0.0407(9) Uani 1 1 d . .
C44 C 0.63290(9) 0.70446(12) 0.87290(8) 0.0376(9) Uani 1 1 d . .
O15 O 0.63396(5) 0.70740(6) 0.81324(5) 0.0245(4) Uani 1 1 d . .
O26 O 0.45200(8) 0.69678(13) 1.03831(8) 0.0651(12) Uani 1 1 d . .
O14 O 0.58564(8) 0.69423(16) 0.83893(8) 0.0860(18) Uani 1 1 d . .
N3 N 0.47641(8) 0.70612(12) 1.08883(8) 0.0487(10) Uani 1 1 d . .
H3 H 0.495425 0.705205 1.099101 0.058 Uiso 1 1 calc R U
C54 C 0.47676(10) 0.70137(14) 1.05496(10) 0.0472(11) Uani 1 1 d . .
C55 C 0.44746(9) 0.71246(13) 1.10873(10) 0.0421(10) Uani 1 1 d . .
C56 C 0.39390(9) 0.72916(10) 1.15066(9) 0.0327(8) Uani 1 1 d . .
H56 H 0.376216 0.735139 1.164754 0.039 Uiso 1 1 calc R U
C57 C 0.39147(8) 0.73441(11) 1.11638(9) 0.0341(8) Uani 1 1 d . .
C58 C 0.44953(10) 0.70651(13) 1.14298(10) 0.0417(10) Uani 1 1 d . .
H58 H 0.468816 0.696856 1.152034 0.050 Uiso 1 1 calc R U
C59 C 0.41824(9) 0.72595(13) 1.09502(9) 0.0415(10) Uani 1 1 d . .
H59 H 0.416468 0.729317 1.071943 0.050 Uiso 1 1 calc R U
C60 C 0.42272(10) 0.71499(12) 1.16385(9) 0.0388(9) Uani 1 1 d . .
C62 C 0.42464(9) 0.70887(11) 1.20096(9) 0.0374(9) Uani 1 1 d . .
C61 C 0.36000(9) 0.74994(11) 1.10194(9) 0.0318(7) Uani 1 1 d . .
O22 O 0.40230(7) 0.72203(7) 1.21851(6) 0.0321(5) Uani 1 1 d . .
O24 O 0.33586(6) 0.75390(7) 1.12098(6) 0.0297(5) Uani 1 1 d . .
O25 O 0.36147(8) 0.75811(12) 1.07150(8) 0.0630(12) Uani 1 1 d . .
O23 O 0.44843(9) 0.69042(14) 1.21126(8) 0.0811(16) Uani 1 1 d . .
O29 O 0.86080(11) 0.76432(9) 0.99591(8) 0.0624(11) Uani 1 1 d . .
C63 C 0.86562(16) 0.79389(15) 0.99614(17) 0.0664(15) Uani 1 1 d . .
H63 H 0.852698 0.806846 0.981560 0.080 Uiso 1 1 calc R U
N5 N 0.8637(3) 0.6448(2) 0.9683(4) 0.170(6) Uani 1 1 d . .
C64 C 0.8548(2) 0.6756(2) 0.9612(2) 0.097(3) Uani 1 1 d . .
H64 H 0.856771 0.682071 0.938824 0.117 Uiso 1 1 calc R U
C66 C 0.8938(3) 0.8465(2) 1.0101(5) 0.204(8) Uani 1 1 d . .
H66A H 0.882184 0.853940 0.990307 0.305 Uiso 1 1 calc R U
H66B H 0.917501 0.850276 1.007454 0.305 Uiso 1 1 calc R U
H66C H 0.885769 0.858726 1.029281 0.305 Uiso 1 1 calc R U
C67 C 0.9125(3) 0.7916(3) 1.0349(2) 0.159(6) Uani 1 1 d . .
H67A H 0.906420 0.792394 1.058217 0.238 Uiso 1 1 calc R U
H67B H 0.934193 0.801727 1.031830 0.238 Uiso 1 1 calc R U
H67C H 0.913194 0.768638 1.027484 0.238 Uiso 1 1 calc R U
C68 C 0.8779(4) 0.6242(4) 0.9392(5) 0.223(10) Uani 1 1 d . .
H68A H 0.860949 0.609262 0.930819 0.335 Uiso 1 1 calc R U
H68B H 0.896868 0.611393 0.946944 0.335 Uiso 1 1 calc R U
H68C H 0.884992 0.639101 0.921529 0.335 Uiso 1 1 calc R U
C69 C 0.8570(6) 0.6332(5) 1.0069(5) 0.292(14) Uani 1 1 d . .
H69A H 0.837003 0.643898 1.015217 0.438 Uiso 1 1 calc R U
H69B H 0.875814 0.639514 1.020622 0.438 Uiso 1 1 calc R U
H69C H 0.854152 0.609188 1.007746 0.438 Uiso 1 1 calc R U
N6 N 0.88757(15) 0.81001(16) 1.01515(16) 0.0812(17) Uani 1 1 d . .
H13 H 0.7761(17) 0.7154(17) 0.9394(17) 0.06(2) Uiso 1 1 d . .
H14 H 0.804(3) 0.7014(18) 0.940(3) 0.18(5) Uiso 1 1 d D .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
O22 Ni1 O24 89.76(11) 12_675 4_567
O22 Ni1 O13 89.43(10) 12_675 .
O24 Ni1 O13 94.78(10) 4_567 .
O22 Ni1 O15 176.33(10) 12_675 45_666
O24 Ni1 O15 92.64(10) 4_567 45_666
O13 Ni1 O15 93.13(9) . 45_666
O22 Ni1 O3 88.34(11) 12_675 .
O24 Ni1 O3 87.15(10) 4_567 .
O13 Ni1 O3 177.05(12) . .
O15 Ni1 O3 89.01(10) 45_666 .
O22 Ni1 O1 90.39(11) 12_675 .
O24 Ni1 O1 174.88(10) 4_567 .
O13 Ni1 O1 90.34(10) . .
O15 Ni1 O1 86.97(10) 45_666 .
O3 Ni1 O1 87.74(11) . .
O25 Ni2 O13 93.45(13) 4_567 .
O25 Ni2 O8 172.6(2) 4_567 .
O13 Ni2 O8 92.19(15) . .
O25 Ni2 O23 91.9(2) 4_567 12_675
O13 Ni2 O23 93.33(13) . 12_675
O8 Ni2 O23 83.0(2) . 12_675
O25 Ni2 O9 87.43(16) 4_567 .
O13 Ni2 O9 90.31(12) . .
O8 Ni2 O9 97.37(15) . .
O23 Ni2 O9 176.33(16) 12_675 .
O25 Ni2 O29 87.35(16) 4_567 .
O13 Ni2 O29 175.08(12) . .
O8 Ni2 O29 87.44(18) . .
O23 Ni2 O29 91.49(15) 12_675 .
O9 Ni2 O29 84.88(14) . .
C39 S1 C31 90.9(2) . .
Ni2 O13 Ni1 117.82(12) . .
C17 O1 Ni1 127.1(2) . .
C64 O9 Ni2 121.2(5) . .
O1 C17 O2 124.4(3) . .
O1 C17 C23 117.3(3) . .
O2 C17 C23 118.3(3) . .
C34 C19 C23 120.7(3) . .
C37 N4 C34 125.6(3) . .
C28 C23 C19 119.4(3) . .
C28 C23 C17 121.1(3) . .
C19 C23 C17 119.5(3) . .
C39 C27 C32 114.3(4) . .
C44 C28 C23 119.7(3) . .
C32 C31 C37 132.7(4) . .
C32 C31 S1 112.2(3) . .
C37 C31 S1 115.1(3) . .
C31 C32 C27 110.8(4) . .
C42 C34 C19 119.7(3) . .
C42 C34 N4 122.4(3) . .
C19 C34 N4 117.8(3) . .
O27 C37 N4 125.2(4) . .
O27 C37 C31 119.4(4) . .
N4 C37 C31 115.3(4) . .
C27 C39 C54 132.5(4) . .
C27 C39 S1 111.7(3) . .
C54 C39 S1 115.7(3) . .
C34 C42 C44 119.5(3) . .
O15 C45 O14 126.1(3) . .
O15 C45 C44 118.2(3) . .
O14 C45 C44 115.7(3) . .
C28 C44 C42 121.0(3) . .
C28 C44 C45 122.1(3) . .
C42 C44 C45 116.8(3) . .
C45 O15 Ni1 124.0(2) . 41_666
C54 N3 C55 125.8(4) . .
O26 C54 N3 124.0(4) . .
O26 C54 C39 121.7(4) . .
N3 C54 C39 114.3(4) . .
C58 C55 C59 120.1(3) . .
C58 C55 N3 118.0(3) . .
C59 C55 N3 121.8(3) . .
C60 C56 C57 119.6(3) . .
C56 C57 C59 120.5(3) . .
C56 C57 C61 119.7(3) . .
C59 C57 C61 119.8(3) . .
C55 C58 C60 120.0(3) . .
C55 C59 C57 119.3(3) . .
C56 C60 C58 120.5(3) . .
C56 C60 C62 118.9(3) . .
C58 C60 C62 120.6(3) . .
O22 C62 O23 126.6(3) . .
O22 C62 C60 116.6(3) . .
O23 C62 C60 116.8(3) . .
O24 C61 O25 126.5(3) . .
O24 C61 C57 117.7(3) . .
O25 C61 C57 115.8(3) . .
C62 O22 Ni1 133.4(2) . 6_467
C61 O24 Ni1 134.8(2) . 4_467
C61 O25 Ni2 129.3(3) . 4_467
C62 O23 Ni2 134.1(3) . 6_467
C63 O29 Ni2 121.0(4) . .
O29 C63 N6 126.1(7) . .
C64 N5 C68 116.1(15) . .
C64 N5 C69 115.2(13) . .
C68 N5 C69 128.7(13) . .
O9 C64 N5 127.3(10) . .
C63 N6 C67 120.8(6) . .
C63 N6 C66 120.5(8) . .
C67 N6 C66 116.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O22 2.009(2) 12_675
Ni1 O24 2.032(2) 4_567
Ni1 O13 2.066(2) .
Ni1 O15 2.068(2) 45_666
Ni1 O3 2.072(2) .
Ni1 O1 2.090(2) .
Ni2 O25 2.003(3) 4_567
Ni2 O13 2.008(2) .
Ni2 O8 2.014(3) .
Ni2 O23 2.020(3) 12_675
Ni2 O9 2.086(3) .
Ni2 O29 2.087(3) .
S1 C39 1.724(4) .
S1 C31 1.726(4) .
O1 C17 1.255(5) .
O9 C64 1.236(9) .
O2 C17 1.261(5) .
C17 C23 1.500(5) .
C19 C34 1.391(5) .
C19 C23 1.396(5) .
N4 C37 1.357(5) .
N4 C34 1.422(5) .
C23 C28 1.390(5) .
C27 C39 1.339(6) .
C27 C32 1.420(5) .
C28 C44 1.381(5) .
C31 C32 1.373(6) .
C31 C37 1.489(5) .
O27 C37 1.220(6) .
C34 C42 1.382(5) .
C39 C54 1.486(5) .
C42 C44 1.396(5) .
C45 O15 1.251(4) .
C45 O14 1.259(5) .
C45 C44 1.512(5) .
O26 C54 1.200(6) .
N3 C54 1.360(5) .
N3 C55 1.419(4) .
C55 C58 1.385(5) .
C55 C59 1.391(5) .
C56 C60 1.381(5) .
C56 C57 1.382(5) .
C57 C59 1.402(5) .
C57 C61 1.509(4) .
C58 C60 1.392(5) .
C60 C62 1.497(5) .
C62 O22 1.245(4) .
C62 O23 1.265(5) .
C61 O24 1.233(4) .
C61 O25 1.255(5) .
O29 C63 1.191(7) .
C63 N6 1.321(7) .
N5 C64 1.305(12) .
N5 C68 1.525(17) .
N5 C69 1.63(2) .
C66 N6 1.484(11) .
C67 N6 1.459(12) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.007 0.001 28815 7833 ' '
