#------------------------------------------------------------------------------
#$Date: 2016-03-05 10:21:40 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177692 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/83/7118388.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_7118388
loop_
_publ_author_name
'Jiang, Xiang'
'Kou, Hui-Zhong'
_publ_section_title
;
 Solid state reconstructive phase transition from porous supramolecular
 network to porous coordination polymer.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2952
_journal_page_last               2955
_journal_paper_doi               10.1039/c5cc09808d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C57 H76 N12 Ni2 O8,8(H2 O)'
_chemical_formula_sum            'C57 H92 N12 Ni2 O16'
_chemical_formula_weight         1318.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2016-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.286(7)
_cell_length_b                   27.286(7)
_cell_length_c                   8.343(3)
_cell_measurement_reflns_used    2162
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.25
_cell_measurement_theta_min      2.55
_cell_volume                     6212(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19465
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.429
_diffrn_reflns_theta_min         1.493
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3539
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.2004
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1655P)²+12.8309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2992
_refine_ls_wR_factor_ref         0.3443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1434
_reflns_number_total             3539
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc09808d2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7118387--7118388.cif.
;
_cod_original_cell_volume        6212(4)
_cod_database_code               7118388
_shelx_shelxl_version_number     2014/7
_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'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
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 0.9924(4) -0.0387(3) 0.2127(11) 0.130(3) Uani 1 1 d . . . A 1
C13 C 0.9670(5) -0.0904(4) 0.2029(17) 0.157(4) Uani 1 1 d . U . A 1
H13A H 0.9842 -0.1106 0.1254 0.188 Uiso 1 1 calc R U . A 1
H13B H 0.9692 -0.1064 0.3064 0.188 Uiso 1 1 calc R U . A 1
C15 C 0.9600(6) -0.0125(5) 0.3150(17) 0.187(7) Uani 1 1 d . . . A 1
H15A H 0.9582 -0.0310 0.4139 0.224 Uiso 1 1 calc R U . A 1
H15B H 0.9764 0.0181 0.3410 0.224 Uiso 1 1 calc R U . A 1
Ni1 Ni 1.0000 0.0000 0.0000 0.0986(7) Uani 1 2 d S . P A 1
O1 O 1.0114(3) 0.06520(17) 0.1272(8) 0.115(2) Uani 1 1 d . U . A 1
O2 O 1.0869(3) 0.0604(2) 0.2407(10) 0.167(3) Uani 1 1 d . . . A 1
C2 C 1.01427(18) 0.20667(16) 0.5110(7) 0.0551(14) Uani 1 1 d . . . A 1
C1 C 1.0000 0.2500 0.6250 0.051(3) Uani 1 4 d S T P A 1
C7 C 1.0578(2) 0.18301(18) 0.5169(9) 0.0717(18) Uani 1 1 d . . . A 1
H7 H 1.0817 0.1934 0.5887 0.086 Uiso 1 1 calc R U . A 1
N1 N 0.9272(3) 0.0204(2) -0.0079(9) 0.117(2) Uani 1 1 d . U . A 1
H1 H 0.9087 -0.0074 -0.0509 0.140 Uiso 1 1 calc R U . A 1
C3 C 0.9814(2) 0.1927(2) 0.3924(9) 0.0767(19) Uani 1 1 d . . . A 1
H3 H 0.9523 0.2100 0.3802 0.092 Uiso 1 1 calc R U . A 1
C5 C 1.0347(3) 0.1282(2) 0.3072(12) 0.099(2) Uani 1 1 d D . . A 1
C6 C 1.0671(2) 0.1433(2) 0.4164(12) 0.095(3) Uani 1 1 d . . . A 1
H6 H 1.0967 0.1267 0.4258 0.114 Uiso 1 1 calc R U . A 1
C8 C 1.0445(5) 0.0809(3) 0.2178(13) 0.129(3) Uani 1 1 d D U . A 1
C4 C 0.9910(3) 0.1542(2) 0.2936(10) 0.092(2) Uani 1 1 d . . . A 1
H4 H 0.9682 0.1452 0.2163 0.110 Uiso 1 1 calc R U . A 1
N3 N 0.9134(6) -0.0006(4) 0.2759(15) 0.187(5) Uani 1 1 d . . . A 1
C10 C 0.9049(5) 0.0335(4) 0.1531(16) 0.153(4) Uani 1 1 d . U . A 1
H10A H 0.9178 0.0650 0.1866 0.184 Uiso 1 1 calc R U . A 1
H10B H 0.8698 0.0372 0.1396 0.184 Uiso 1 1 calc R U . A 1
C14 C 0.9153(6) -0.0863(4) 0.156(2) 0.172(5) Uani 1 1 d . U . A 1
H14A H 0.9000 -0.1182 0.1672 0.207 Uiso 1 1 calc R U . A 1
H14B H 0.9137 -0.0772 0.0438 0.207 Uiso 1 1 calc R U . A 1
C12 C 0.9600(6) 0.0498(4) -0.2611(13) 0.159(5) Uani 1 1 d . . . A 1
H12A H 0.9473 0.0221 -0.3212 0.191 Uiso 1 1 calc R U . A 1
H12B H 0.9615 0.0775 -0.3338 0.191 Uiso 1 1 calc R U . A 1
C11 C 0.9240(4) 0.0617(3) -0.1302(16) 0.142(4) Uani 1 1 d . . . A 1
H11A H 0.8911 0.0640 -0.1734 0.170 Uiso 1 1 calc R U . A 1
H11B H 0.9323 0.0928 -0.0806 0.170 Uiso 1 1 calc R U . A 1
C9 C 0.8858(6) -0.0493(6) 0.253(2) 0.207(7) Uani 1 1 d . U . A 1
H9A H 0.8783 -0.0631 0.3567 0.249 Uiso 1 1 calc R U . A 1
H9B H 0.8551 -0.0429 0.1980 0.249 Uiso 1 1 calc R U . A 1
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'
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
C12 N2 C15 121.0(12) 9_755 .
C12 N2 C13 103.3(8) 9_755 .
C15 N2 C13 102.0(10) . .
C12 N2 Ni1 105.4(7) 9_755 .
C15 N2 Ni1 108.7(7) . .
C13 N2 Ni1 117.1(8) . .
C14 C13 N2 111.6(9) . .
C14 C13 H13A 109.3 . .
N2 C13 H13A 109.3 . .
C14 C13 H13B 109.3 . .
N2 C13 H13B 109.3 . .
H13A C13 H13B 108.0 . .
N3 C15 N2 124.1(15) . .
N3 C15 H15A 106.3 . .
N2 C15 H15A 106.3 . .
N3 C15 H15B 106.3 . .
N2 C15 H15B 106.3 . .
H15A C15 H15B 106.4 . .
N1 Ni1 N1 180.0 . 9_755
N1 Ni1 N2 86.1(3) . 9_755
N1 Ni1 N2 93.9(3) 9_755 9_755
N1 Ni1 N2 93.9(3) . .
N1 Ni1 N2 86.1(3) 9_755 .
N2 Ni1 N2 180.0 9_755 .
N1 Ni1 O1 86.0(3) . .
N1 Ni1 O1 94.0(3) 9_755 .
N2 Ni1 O1 89.2(3) 9_755 .
N2 Ni1 O1 90.8(3) . .
N1 Ni1 O1 94.0(3) . 9_755
N1 Ni1 O1 86.0(3) 9_755 9_755
N2 Ni1 O1 90.8(3) 9_755 9_755
N2 Ni1 O1 89.2(3) . 9_755
O1 Ni1 O1 180.0 . 9_755
C8 O1 Ni1 134.7(6) . .
C7 C2 C3 117.5(5) . .
C7 C2 C1 123.8(5) . .
C3 C2 C1 118.6(4) . .
C2 C1 C2 105.2(4) 12_757 14_666
C2 C1 C2 111.6(2) 12_757 7_654
C2 C1 C2 111.6(2) 14_666 7_654
C2 C1 C2 111.6(2) 12_757 .
C2 C1 C2 111.6(2) 14_666 .
C2 C1 C2 105.2(4) 7_654 .
C2 C7 C6 120.6(6) . .
C2 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C10 N1 C11 113.3(7) . .
C10 N1 Ni1 114.9(7) . .
C11 N1 Ni1 106.0(6) . .
C10 N1 H1 107.4 . .
C11 N1 H1 107.4 . .
Ni1 N1 H1 107.4 . .
C4 C3 C2 121.2(6) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C6 C5 C4 117.8(6) . .
C6 C5 C8 118.8(9) . .
C4 C5 C8 123.1(9) . .
C5 C6 C7 122.0(6) . .
C5 C6 H6 119.0 . .
C7 C6 H6 119.0 . .
O1 C8 O2 125.7(7) . .
O1 C8 C5 117.5(10) . .
O2 C8 C5 116.8(10) . .
C3 C4 C5 120.6(7) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C15 N3 C10 119.4(13) . .
C15 N3 C9 106.5(11) . .
C10 N3 C9 113.5(15) . .
N3 C10 N1 115.1(8) . .
N3 C10 H10A 108.5 . .
N1 C10 H10A 108.5 . .
N3 C10 H10B 108.5 . .
N1 C10 H10B 108.5 . .
H10A C10 H10B 107.5 . .
C13 C14 C9 114.7(14) . .
C13 C14 H14A 108.6 . .
C9 C14 H14A 108.6 . .
C13 C14 H14B 108.6 . .
C9 C14 H14B 108.6 . .
H14A C14 H14B 107.6 . .
N2 C12 C11 116.4(10) 9_755 .
N2 C12 H12A 108.2 9_755 .
C11 C12 H12A 108.2 . .
N2 C12 H12B 108.2 9_755 .
C11 C12 H12B 108.2 . .
H12A C12 H12B 107.3 . .
C12 C11 N1 106.7(7) . .
C12 C11 H11A 110.4 . .
N1 C11 H11A 110.4 . .
C12 C11 H11B 110.4 . .
N1 C11 H11B 110.4 . .
H11A C11 H11B 108.6 . .
C14 C9 N3 112.4(11) . .
C14 C9 H9A 109.1 . .
N3 C9 H9A 109.1 . .
C14 C9 H9B 109.1 . .
N3 C9 H9B 109.1 . .
H9A C9 H9B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N2 C12 1.393(14) 9_755
N2 C15 1.421(15) .
N2 C13 1.575(14) .
N2 Ni1 2.075(8) .
C13 C14 1.468(16) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C15 N3 1.353(18) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
Ni1 N1 2.063(8) .
Ni1 N1 2.063(8) 9_755
Ni1 N2 2.074(8) 9_755
Ni1 O1 2.095(5) .
Ni1 O1 2.095(5) 9_755
O1 C8 1.251(12) .
O2 C8 1.300(13) .
C2 C7 1.352(7) .
C2 C3 1.388(8) .
C2 C1 1.567(5) .
C1 C2 1.567(5) 12_757
C1 C2 1.567(5) 14_666
C1 C2 1.567(5) 7_654
C7 C6 1.394(10) .
C7 H7 0.9300 .
N1 C10 1.518(13) .
N1 C11 1.524(12) .
N1 H1 0.9800 .
C3 C4 1.361(9) .
C3 H3 0.9300 .
C5 C6 1.334(12) .
C5 C4 1.391(10) .
C5 C8 1.515(8) .
C6 H6 0.9300 .
C4 H4 0.9300 .
N3 C10 1.403(15) .
N3 C9 1.539(19) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C14 C9 1.521(18) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C12 N2 1.393(14) 9_755
C12 C11 1.504(15) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
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_4
C12 N2 C13 C14 178.8(11) 9_755 .
C15 N2 C13 C14 52.6(14) . .
Ni1 N2 C13 C14 -65.9(12) . .
C12 N2 C15 N3 -179.8(12) 9_755 .
C13 N2 C15 N3 -66.1(15) . .
Ni1 N2 C15 N3 58.2(16) . .
C7 C2 C1 C2 3.3(5) . 12_757
C3 C2 C1 C2 -174.1(5) . 12_757
C7 C2 C1 C2 -114.2(6) . 14_666
C3 C2 C1 C2 68.5(4) . 14_666
C7 C2 C1 C2 124.6(5) . 7_654
C3 C2 C1 C2 -52.8(4) . 7_654
C3 C2 C7 C6 -5.6(8) . .
C1 C2 C7 C6 177.0(5) . .
C7 C2 C3 C4 4.9(9) . .
C1 C2 C3 C4 -177.6(6) . .
C4 C5 C6 C7 1.3(12) . .
C8 C5 C6 C7 -172.0(7) . .
C2 C7 C6 C5 2.6(11) . .
Ni1 O1 C8 O2 10.2(18) . .
Ni1 O1 C8 C5 -170.7(6) . .
C6 C5 C8 O1 173.4(9) . .
C4 C5 C8 O1 0.5(15) . .
C6 C5 C8 O2 -7.4(14) . .
C4 C5 C8 O2 179.7(9) . .
C2 C3 C4 C5 -1.1(11) . .
C6 C5 C4 C3 -2.0(12) . .
C8 C5 C4 C3 171.0(8) . .
N2 C15 N3 C10 -67(2) . .
N2 C15 N3 C9 62.7(16) . .
C15 N3 C10 N1 57.2(19) . .
C9 N3 C10 N1 -69.7(15) . .
C11 N1 C10 N3 -171.0(12) . .
Ni1 N1 C10 N3 -48.9(14) . .
N2 C13 C14 C9 -49.9(15) . .
N2 C12 C11 N1 -51.3(13) 9_755 .
C10 N1 C11 C12 163.1(10) . .
Ni1 N1 C11 C12 36.2(10) . .
C13 C14 C9 N3 44.7(17) . .
C15 N3 C9 C14 -44.1(17) . .
C10 N3 C9 C14 89.3(15) . .
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 0.250 0.500 0.599 299 72 ' '
2 0.250 1.000 0.391 299 72 ' '
3 0.750 0.500 0.891 299 72 ' '
4 0.750 1.000 0.099 299 72 ' '
