#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:38:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179120 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/82/4308271.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_4308271
loop_
_publ_author_name
'Shengqian Ma'
'Xi-Sen Wang'
'Erika S. Manis'
'Christopher D. Collier'
'Hong-Cai Zhou'
_publ_section_title
;
Metal-Organic Framework Based on a Trinickel Secondary Building Unit
Exhibiting Gas-Sorption Hysteresis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3432
_journal_page_last               3434
_journal_paper_doi               10.1021/ic070338v
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'Ni3 O (C24H12N3O6)2 (H2O)3'
_chemical_formula_sum            'C48 H30 N6 Ni3 O16'
_chemical_formula_weight         1122.91
_chemical_melting_point          ?
_chemical_name_common            PCN-5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 123.188(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.175(3)
_cell_length_b                   21.108(3)
_cell_length_c                   16.762(2)
_cell_measurement_reflns_used    6180
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.84
_cell_measurement_theta_min      2.23
_cell_volume                     8934.8(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25322
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'LIGHT GREEN'
_exptl_crystal_density_diffrn    0.835
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         8083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0476
_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)+(0.0731P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                5776
_reflns_number_total             8083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070338v-file002.cif
_cod_data_source_block           sq
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8934.7(18)
_cod_database_code               4308271
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'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.100347(15) 0.5000 0.02915(3) 0.03112(13) Uani 1 2 d S . .
Ni2 Ni 0.223086(18) 0.5000 0.04689(3) 0.04847(16) Uani 1 2 d S . .
Ni3 Ni 0.101305(17) 0.5000 -0.17436(3) 0.04813(16) Uani 1 2 d S . .
O1 O 0.14963(7) 0.43187(10) 0.12656(14) 0.0583(6) Uani 1 1 d . . .
O10 O 0.05849(14) 0.5000 -0.3247(2) 0.1148(17) Uani 1 2 d S . .
O2 O 0.22715(9) 0.43095(13) 0.13918(16) 0.0752(7) Uani 1 1 d . . .
O12 O 0.06228(11) 0.5000 0.1045(2) 0.0635(8) Uani 1 2 d S . .
O3 O 0.04737(7) 0.43138(9) -0.05869(13) 0.0524(5) Uani 1 1 d . . .
O11 O 0.30810(17) 0.5000 0.1311(3) 0.154(2) Uani 1 2 d S . .
O4 O 0.05058(9) 0.42972(13) -0.18803(16) 0.0773(7) Uani 1 1 d . . .
O5 O 0.14886(8) 0.43214(13) -0.17792(17) 0.0779(7) Uani 1 1 d . . .
O6 O 0.22728(9) 0.43179(12) -0.03793(15) 0.0675(6) Uani 1 1 d . . .
O7 O 0.14273(7) 0.5000 -0.03099(13) 0.0257(5) Uani 1 2 d S . .
N1 N 0.33523(10) 0.27830(12) 0.58743(17) 0.0564(7) Uani 1 1 d . . .
N2 N 0.33551(10) 0.27920(13) 0.72949(17) 0.0616(7) Uani 1 1 d . . .
N3 N 0.26692(10) 0.33151(13) 0.59047(18) 0.0607(7) Uani 1 1 d . . .
C1 C 0.19733(12) 0.41949(14) 0.1680(2) 0.0489(7) Uani 1 1 d . . .
C2 C 0.22153(11) 0.38826(15) 0.26482(19) 0.0503(7) Uani 1 1 d . . .
C3 C 0.26934(13) 0.35413(18) 0.3077(2) 0.0717(11) Uani 1 1 d . . .
H3 H 0.2864 0.3492 0.2758 0.086 Uiso 1 1 calc R . .
C4 C 0.29121(13) 0.32761(17) 0.3983(2) 0.0684(10) Uani 1 1 d . . .
H4 H 0.3218 0.3033 0.4252 0.082 Uiso 1 1 calc R . .
C5 C 0.26733(12) 0.33762(15) 0.4476(2) 0.0547(8) Uani 1 1 d . . .
C6 C 0.21975(14) 0.36988(18) 0.4033(2) 0.0693(10) Uani 1 1 d . . .
H6 H 0.2027 0.3750 0.4353 0.083 Uiso 1 1 calc R . .
C7 C 0.19688(12) 0.39456(17) 0.3132(2) 0.0637(9) Uani 1 1 d . . .
H7 H 0.1646 0.4156 0.2848 0.076 Uiso 1 1 calc R . .
C8 C 0.29119(12) 0.31354(14) 0.5470(2) 0.0525(7) Uani 1 1 d . . .
C9 C 0.03251(10) 0.41281(14) -0.1398(2) 0.0474(7) Uani 1 1 d . . .
C10 C 0.26639(13) 0.33640(15) -0.2673(2) 0.0586(8) Uani 1 1 d . . .
C11 C 0.29411(16) 0.3372(2) -0.1692(2) 0.0829(12) Uani 1 1 d . . .
H11 H 0.3280 0.3200 -0.1336 0.099 Uiso 1 1 calc R . .
C12 C -0.07862(14) 0.30442(17) -0.1837(2) 0.0703(10) Uani 1 1 d . . .
H12 H -0.0945 0.2924 -0.1517 0.084 Uiso 1 1 calc R . .
C13 C 0.40213(12) 0.21900(16) 0.7264(2) 0.0575(8) Uani 1 1 d . . .
C14 C -0.07466(15) 0.3010(2) -0.3203(3) 0.0959(15) Uani 1 1 d . . .
H14 H -0.0877 0.2868 -0.3819 0.115 Uiso 1 1 calc R . .
C15 C -0.03166(16) 0.3425(2) -0.2764(3) 0.1044(17) Uani 1 1 d . . .
H15 H -0.0160 0.3551 -0.3086 0.125 Uiso 1 1 calc R . .
C16 C 0.35499(12) 0.26149(15) 0.6782(2) 0.0546(8) Uani 1 1 d . . .
C17 C 0.19704(13) 0.42032(16) -0.1251(2) 0.0584(8) Uani 1 1 d . . .
C18 C 0.22114(13) 0.38866(16) -0.1740(2) 0.0584(8) Uani 1 1 d . . .
C19 C 0.19318(15) 0.3849(2) -0.2711(3) 0.0935(14) Uani 1 1 d . . .
H19 H 0.1587 0.4003 -0.3066 0.112 Uiso 1 1 calc R . .
C20 C 0.27189(15) 0.3636(2) -0.1232(2) 0.0821(12) Uani 1 1 d . . .
H20 H 0.2914 0.3645 -0.0569 0.098 Uiso 1 1 calc R . .
C21 C 0.21500(16) 0.3586(3) -0.3184(3) 0.1027(17) Uani 1 1 d . . .
H21 H 0.1949 0.3561 -0.3846 0.123 Uiso 1 1 calc R . .
C22 C -0.03645(13) 0.34522(16) -0.1406(2) 0.0660(9) Uani 1 1 d . . .
H22 H -0.0240 0.3599 -0.0795 0.079 Uiso 1 1 calc R . .
C23 C -0.01207(10) 0.36504(14) -0.1861(2) 0.0482(7) Uani 1 1 d . . .
C24 C 0.29020(13) 0.31351(16) 0.6809(2) 0.0579(8) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
_geom_angle_publ_flag
O7 Ni1 O3 95.69(7) . . ?
O7 Ni1 O3 95.69(7) . 6_565 ?
O3 Ni1 O3 89.34(12) . 6_565 ?
O7 Ni1 O1 90.91(7) . 6_565 ?
O3 Ni1 O1 173.33(8) . 6_565 ?
O3 Ni1 O1 90.95(9) 6_565 6_565 ?
O7 Ni1 O1 90.91(7) . . ?
O3 Ni1 O1 90.95(9) . . ?
O3 Ni1 O1 173.33(8) 6_565 . ?
O1 Ni1 O1 87.98(13) 6_565 . ?
O7 Ni1 O12 174.87(9) . . ?
O3 Ni1 O12 87.94(8) . . ?
O3 Ni1 O12 87.94(8) 6_565 . ?
O1 Ni1 O12 85.40(8) 6_565 . ?
O1 Ni1 O12 85.40(8) . . ?
O7 Ni2 O6 93.36(7) . . ?
O7 Ni2 O6 93.36(7) . 6_565 ?
O6 Ni2 O6 87.85(14) . 6_565 ?
O7 Ni2 O2 92.39(7) . 6_565 ?
O6 Ni2 O2 174.22(9) . 6_565 ?
O6 Ni2 O2 91.29(10) 6_565 6_565 ?
O7 Ni2 O2 92.39(7) . . ?
O6 Ni2 O2 91.29(10) . . ?
O6 Ni2 O2 174.22(9) 6_565 . ?
O2 Ni2 O2 89.00(15) 6_565 . ?
O7 Ni2 O11 179.19(15) . . ?
O6 Ni2 O11 87.22(12) . . ?
O6 Ni2 O11 87.22(12) 6_565 . ?
O2 Ni2 O11 87.03(12) 6_565 . ?
O2 Ni2 O11 87.03(12) . . ?
O7 Ni3 O5 92.73(8) . 6_565 ?
O7 Ni3 O5 92.73(8) . . ?
O5 Ni3 O5 88.57(15) 6_565 . ?
O7 Ni3 O4 94.08(8) . 6_565 ?
O5 Ni3 O4 89.02(11) 6_565 6_565 ?
O5 Ni3 O4 172.88(10) . 6_565 ?
O7 Ni3 O4 94.08(8) . . ?
O5 Ni3 O4 172.88(10) 6_565 . ?
O5 Ni3 O4 89.02(11) . . ?
O4 Ni3 O4 92.58(15) 6_565 . ?
O7 Ni3 O10 179.49(12) . . ?
O5 Ni3 O10 86.91(10) 6_565 . ?
O5 Ni3 O10 86.91(10) . . ?
O4 Ni3 O10 86.27(10) 6_565 . ?
O4 Ni3 O10 86.27(10) . . ?
C1 O1 Ni1 134.67(19) . . ?
C1 O2 Ni2 131.16(19) . . ?
C9 O3 Ni1 132.79(19) . . ?
C9 O4 Ni3 134.22(19) . . ?
C17 O5 Ni3 133.0(2) . . ?
C17 O6 Ni2 130.9(2) . . ?
Ni3 O7 Ni1 116.60(9) . . ?
Ni3 O7 Ni2 120.72(10) . . ?
Ni1 O7 Ni2 122.69(9) . . ?
C8 N1 C16 115.0(3) . . ?
C16 N2 C24 114.7(2) . . ?
C24 N3 C8 115.7(2) . . ?
O1 C1 O2 127.0(3) . . ?
O1 C1 C2 115.1(3) . . ?
O2 C1 C2 117.9(2) . . ?
C7 C2 C3 118.8(3) . . ?
C7 C2 C1 119.3(2) . . ?
C3 C2 C1 121.8(3) . . ?
C4 C3 C2 120.2(3) . . ?
C5 C4 C3 119.9(3) . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 C8 121.7(3) . . ?
C6 C5 C8 119.4(3) . . ?
C7 C6 C5 121.8(3) . . ?
C6 C7 C2 120.2(3) . . ?
N1 C8 N3 124.7(3) . . ?
N1 C8 C5 119.4(3) . . ?
N3 C8 C5 115.9(2) . . ?
O3 C9 O4 126.6(3) . . ?
O3 C9 C23 117.3(3) . . ?
O4 C9 C23 116.1(3) . . ?
C11 C10 C21 118.6(3) . . ?
C11 C10 C24 122.2(3) . 1_554 ?
C21 C10 C24 119.3(3) . 1_554 ?
C10 C11 C20 120.5(3) . . ?
C22 C12 C13 121.1(3) . 8_454 ?
C14 C13 C12 118.2(3) 8_556 8_556 ?
C14 C13 C16 120.6(3) 8_556 . ?
C12 C13 C16 121.0(3) 8_556 . ?
C13 C14 C15 120.6(3) 8_454 . ?
C23 C15 C14 121.0(3) . . ?
N2 C16 N1 125.3(2) . . ?
N2 C16 C13 116.5(2) . . ?
N1 C16 C13 118.2(3) . . ?
O5 C17 O6 127.7(3) . . ?
O5 C17 C18 115.0(3) . . ?
O6 C17 C18 117.2(3) . . ?
C19 C18 C20 117.7(3) . . ?
C19 C18 C17 120.2(3) . . ?
C20 C18 C17 122.1(3) . . ?
C18 C19 C21 121.7(3) . . ?
C11 C20 C18 121.2(3) . . ?
C10 C21 C19 120.2(3) . . ?
C12 C22 C23 121.4(3) . . ?
C15 C23 C22 117.7(3) . . ?
C15 C23 C9 121.4(3) . . ?
C22 C23 C9 120.8(3) . . ?
N3 C24 N2 124.5(3) . . ?
N3 C24 C10 116.9(3) . 1_556 ?
N2 C24 C10 118.4(3) . 1_556 ?
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 O7 2.016(2) . ?
Ni1 O3 2.0602(17) . ?
Ni1 O3 2.0602(17) 6_565 ?
Ni1 O1 2.0707(18) 6_565 ?
Ni1 O1 2.0707(18) . ?
Ni1 O12 2.121(3) . ?
Ni2 O7 2.0292(19) . ?
Ni2 O6 2.075(2) . ?
Ni2 O6 2.075(2) 6_565 ?
Ni2 O2 2.080(2) 6_565 ?
Ni2 O2 2.080(2) . ?
Ni2 O11 2.147(4) . ?
Ni3 O7 2.0121(19) . ?
Ni3 O5 2.051(2) 6_565 ?
Ni3 O5 2.051(2) . ?
Ni3 O4 2.052(2) 6_565 ?
Ni3 O4 2.052(2) . ?
Ni3 O10 2.110(3) . ?
O1 C1 1.236(3) . ?
O2 C1 1.257(4) . ?
O3 C9 1.240(3) . ?
O4 C9 1.249(4) . ?
O5 C17 1.245(4) . ?
O6 C17 1.252(4) . ?
N1 C8 1.339(3) . ?
N1 C16 1.343(3) . ?
N2 C16 1.333(4) . ?
N2 C24 1.356(4) . ?
N3 C24 1.330(4) . ?
N3 C8 1.340(4) . ?
C1 C2 1.517(4) . ?
C2 C7 1.374(4) . ?
C2 C3 1.408(4) . ?
C3 C4 1.398(4) . ?
C4 C5 1.378(4) . ?
C5 C6 1.382(4) . ?
C5 C8 1.497(4) . ?
C6 C7 1.374(4) . ?
C9 C23 1.512(4) . ?
C10 C11 1.378(4) . ?
C10 C21 1.380(5) . ?
C10 C24 1.478(4) 1_554 ?
C11 C20 1.386(5) . ?
C12 C22 1.370(4) . ?
C12 C13 1.375(4) 8_454 ?
C13 C14 1.373(5) 8_556 ?
C13 C12 1.375(4) 8_556 ?
C13 C16 1.491(4) . ?
C14 C13 1.373(5) 8_454 ?
C14 C15 1.395(5) . ?
C15 C23 1.373(4) . ?
C17 C18 1.517(4) . ?
C18 C19 1.365(5) . ?
C18 C20 1.387(4) . ?
C19 C21 1.393(5) . ?
C22 C23 1.382(4) . ?
C24 C10 1.478(4) 1_556 ?
