#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/19/4301901.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_4301901
loop_
_publ_author_name
'Louise N. Dawe'
'Konstantin V. Shuvaev'
'Laurence K. Thompson'
_publ_section_title
;
Magnetic [nxn] (n= 2-5) Grids by Directed Self-Assembly
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3323
_journal_page_last               3341
_journal_paper_doi               10.1021/ic801078h
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C53.2 H72.8 N28 Ni4 O25.2'
_chemical_formula_weight         1742.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 113.239(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.508(4)
_cell_length_b                   16.6429(18)
_cell_length_c                   16.857(2)
_cell_measurement_reflns_used    11308
_cell_measurement_temperature    138(2)
_cell_measurement_theta_max      30.8140
_cell_measurement_theta_min      2.3546
_cell_volume                     7606.8(16)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      138(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32733
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.8253
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3606.40
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.33
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 345.6 electrons per
unit cell in one void (2685.4 A3), that is 172.8 electrons per
formula unit. Disordered solvent methanol appeared to be present prior to the 
application of Squeeze, though a good point atom model could not be achieved
for these. The application of squeeze gave a good improvement in the data 
statistics and allowed for a full refinement of the framework structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00045(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1092P)²+3.9525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1866
_reflns_number_gt                6582
_reflns_number_total             7881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801078h_si_001_1.cif
_cod_data_source_block           shelxl_(3)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C53.20 H72.80 N28 O25.20 Ni4'
_cod_database_code               4301901
loop_
_symmetry_equiv_pos_as_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'
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 0.100369(15) 0.75715(2) 0.31563(3) 0.04148(16) Uani 1 1 d . . .
Ni2 Ni 0.002020(15) 0.751105(19) 0.41837(3) 0.04201(16) Uani 1 1 d . . .
O1 O -0.11179(9) 1.08369(15) 0.44049(17) 0.0642(6) Uani 1 1 d . . .
O2 O -0.13105(10) 0.95769(16) 0.46053(19) 0.0689(7) Uani 1 1 d . . .
O3 O 0.04768(7) 0.79891(12) 0.36335(12) 0.0431(5) Uani 1 1 d . . .
O4 O -0.10913(9) 0.40939(14) -0.08014(18) 0.0688(7) Uani 1 1 d . . .
O5 O -0.13355(11) 0.53256(17) -0.12788(18) 0.0789(8) Uani 1 1 d . . .
O6 O 0.04658(7) 0.70944(12) 0.20018(12) 0.0428(5) Uani 1 1 d . . .
O7 O 0.05453(9) 0.77809(14) 0.54069(14) 0.0545(6) Uani 1 1 d . . .
O8 O -0.04695(9) 0.72050(14) 0.47343(16) 0.0564(6) Uani 1 1 d . . .
N1 N -0.05612(9) 0.89960(15) 0.42518(16) 0.0461(6) Uani 1 1 d . . .
N2 N -0.02004(9) 0.87083(14) 0.40403(15) 0.0427(5) Uani 1 1 d . . .
N3 N 0.07016(9) 0.92276(14) 0.32552(16) 0.0442(6) Uani 1 1 d . . .
N4 N 0.10124(9) 0.87432(15) 0.30175(16) 0.0426(6) Uani 1 1 d . . .
N5 N 0.14235(10) 0.98770(15) 0.28218(18) 0.0525(6) Uani 1 1 d . . .
H3 H 0.1246 1.0207 0.2991 0.063 Uiso 1 1 calc R . .
H4 H 0.1654 1.0068 0.2666 0.063 Uiso 1 1 calc R . .
N6 N 0.21749(12) 0.8176(2) 0.1846(2) 0.0666(8) Uani 1 1 d . . .
N7 N 0.15150(10) 0.77326(16) 0.25764(17) 0.0460(6) Uani 1 1 d . . .
N8 N -0.05830(9) 0.59855(15) 0.00490(16) 0.0448(6) Uani 1 1 d . . .
N9 N -0.02199(9) 0.63111(14) 0.07354(15) 0.0418(5) Uani 1 1 d . . .
N10 N 0.07382(9) 0.58899(14) 0.27470(16) 0.0421(5) Uani 1 1 d . . .
N11 N 0.10529(9) 0.64119(14) 0.33733(16) 0.0419(5) Uani 1 1 d . . .
N12 N 0.14711(10) 0.53220(15) 0.42012(17) 0.0495(6) Uani 1 1 d . . .
H10 H 0.1285 0.4971 0.3822 0.059 Uiso 1 1 calc R . .
H11 H 0.1710 0.5155 0.4679 0.059 Uiso 1 1 calc R . .
N13 N 0.23260(12) 0.7140(2) 0.5993(2) 0.0679(9) Uani 1 1 d . . .
N14 N 0.15729(11) 0.74848(14) 0.44112(18) 0.0464(6) Uani 1 1 d . . .
C1 C -0.10558(12) 1.0096(2) 0.4427(2) 0.0531(8) Uani 1 1 d . . .
C2 C -0.06406(11) 0.97851(18) 0.41884(19) 0.0454(7) Uani 1 1 d . . .
C3 C -0.03710(12) 1.03119(18) 0.3902(2) 0.0486(7) Uani 1 1 d . . .
H1 H -0.0441 1.0871 0.3856 0.058 Uiso 1 1 calc R . .
C4 C -0.00086(11) 1.00141(17) 0.3690(2) 0.0450(7) Uani 1 1 d . . .
H2 H 0.0185 1.0355 0.3497 0.054 Uiso 1 1 calc R . .
C5 C 0.00705(10) 0.91827(16) 0.37668(18) 0.0405(6) Uani 1 1 d . . .
C6 C 0.04414(10) 0.87705(17) 0.35451(18) 0.0425(6) Uani 1 1 d . . .
C7 C 0.13429(11) 0.90923(18) 0.28017(19) 0.0451(7) Uani 1 1 d . . .
C8 C 0.16221(11) 0.85131(18) 0.25072(19) 0.0454(7) Uani 1 1 d . . .
C9 C 0.19599(13) 0.8717(2) 0.2158(2) 0.0572(8) Uani 1 1 d . . .
H5 H 0.2041 0.9268 0.2142 0.069 Uiso 1 1 calc R . .
C10 C 0.20584(16) 0.7415(2) 0.1911(3) 0.0626(10) Uani 1 1 d . . .
H6 H 0.2209 0.7009 0.1703 0.075 Uiso 1 1 calc R . .
C11 C 0.17330(12) 0.7186(2) 0.2262(2) 0.0558(8) Uani 1 1 d . . .
H7 H 0.1660 0.6633 0.2283 0.067 Uiso 1 1 calc R . .
C12 C -0.10537(12) 0.4836(2) -0.0751(2) 0.0566(8) Uani 1 1 d . . .
C13 C -0.06364(11) 0.51929(17) 0.0031(2) 0.0443(6) Uani 1 1 d . . .
C14 C -0.03330(11) 0.46824(17) 0.0685(2) 0.0448(7) Uani 1 1 d . . .
H8 H -0.0381 0.4117 0.0646 0.054 Uiso 1 1 calc R . .
C15 C 0.00351(11) 0.50226(17) 0.1381(2) 0.0423(6) Uani 1 1 d . . .
H9 H 0.0252 0.4706 0.1844 0.051 Uiso 1 1 calc R . .
C16 C 0.00764(10) 0.58634(16) 0.13766(19) 0.0398(6) Uani 1 1 d . . .
C17 C 0.04532(10) 0.63163(17) 0.20874(18) 0.0421(6) Uani 1 1 d . . .
C18 C 0.13922(10) 0.61010(17) 0.40522(19) 0.0427(6) Uani 1 1 d . . .
C19 C 0.16881(11) 0.67159(18) 0.46783(19) 0.0446(6) Uani 1 1 d . . .
C20 C 0.20671(13) 0.6554(2) 0.5468(2) 0.0607(9) Uani 1 1 d . . .
H12 H 0.2145 0.6010 0.5641 0.073 Uiso 1 1 calc R . .
C21 C 0.22045(14) 0.7889(2) 0.5735(2) 0.0624(9) Uani 1 1 d . . .
H13 H 0.2383 0.8317 0.6098 0.075 Uiso 1 1 calc R . .
C22 C 0.18216(12) 0.8069(2) 0.4946(2) 0.0540(8) Uani 1 1 d . . .
H14 H 0.1738 0.8614 0.4789 0.065 Uiso 1 1 calc R . .
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
_geom_angle_publ_flag
N11 Ni1 N4 175.01(10) . . ?
N11 Ni1 N7 101.39(11) . . ?
N4 Ni1 N7 76.93(10) . . ?
N11 Ni1 O6 77.06(9) . . ?
N4 Ni1 O6 107.60(9) . . ?
N7 Ni1 O6 92.04(9) . . ?
N11 Ni1 N14 77.05(9) . . ?
N4 Ni1 N14 98.25(9) . . ?
N7 Ni1 N14 92.34(11) . . ?
O6 Ni1 N14 154.10(8) . . ?
N11 Ni1 O3 105.21(10) . . ?
N4 Ni1 O3 76.52(9) . . ?
N7 Ni1 O3 153.40(9) . . ?
O6 Ni1 O3 94.31(8) . . ?
N14 Ni1 O3 93.11(10) . . ?
O8 Ni2 O6 90.59(9) . 2 ?
O8 Ni2 N9 87.93(10) . 2 ?
O6 Ni2 N9 79.10(9) 2 2 ?
O8 Ni2 O3 171.62(9) . . ?
O6 Ni2 O3 91.24(8) 2 . ?
N9 Ni2 O3 100.45(9) 2 . ?
O8 Ni2 N2 92.64(10) . . ?
O6 Ni2 N2 98.23(8) 2 . ?
N9 Ni2 N2 177.28(9) 2 . ?
O3 Ni2 N2 79.00(9) . . ?
O8 Ni2 O7 89.28(10) . . ?
O6 Ni2 O7 172.63(8) 2 . ?
N9 Ni2 O7 93.53(9) 2 . ?
O3 Ni2 O7 89.95(9) . . ?
N2 Ni2 O7 89.14(9) . . ?
C6 O3 Ni2 113.31(18) . . ?
C6 O3 Ni1 108.58(18) . . ?
Ni2 O3 Ni1 138.10(10) . . ?
C17 O6 Ni2 113.62(16) . 2 ?
C17 O6 Ni1 108.28(16) . . ?
Ni2 O6 Ni1 138.09(10) 2 . ?
C2 N1 N2 117.7(3) . . ?
C5 N2 N1 122.1(2) . . ?
C5 N2 Ni2 113.95(19) . . ?
N1 N2 Ni2 123.88(19) . . ?
C6 N3 N4 108.8(2) . . ?
C7 N4 N3 118.2(2) . . ?
C7 N4 Ni1 121.4(2) . . ?
N3 N4 Ni1 119.93(19) . . ?
C9 N6 C10 115.8(3) . . ?
C11 N7 C8 117.0(3) . . ?
C11 N7 Ni1 129.7(3) . . ?
C8 N7 Ni1 113.3(2) . . ?
C13 N8 N9 117.9(2) . . ?
C16 N9 N8 121.6(2) . . ?
C16 N9 Ni2 114.27(18) . 2 ?
N8 N9 Ni2 123.74(18) . 2 ?
C17 N10 N11 108.5(2) . . ?
C18 N11 N10 118.1(2) . . ?
C18 N11 Ni1 122.2(2) . . ?
N10 N11 Ni1 119.51(17) . . ?
C21 N13 C20 117.5(3) . . ?
C22 N14 C19 117.7(3) . . ?
C22 N14 Ni1 129.2(2) . . ?
C19 N14 Ni1 113.0(2) . . ?
O1 C1 O2 126.3(3) . . ?
O1 C1 C2 116.9(3) . . ?
O2 C1 C2 116.7(3) . . ?
N1 C2 C3 122.9(3) . . ?
N1 C2 C1 116.7(3) . . ?
C3 C2 C1 120.5(3) . . ?
C4 C3 C2 118.8(3) . . ?
C3 C4 C5 117.4(3) . . ?
N2 C5 C4 121.2(3) . . ?
N2 C5 C6 115.1(2) . . ?
C4 C5 C6 123.7(3) . . ?
N3 C6 O3 126.1(3) . . ?
N3 C6 C5 115.7(3) . . ?
O3 C6 C5 118.2(3) . . ?
N4 C7 N5 125.3(3) . . ?
N4 C7 C8 112.4(3) . . ?
N5 C7 C8 122.3(3) . . ?
N7 C8 C9 120.2(3) . . ?
N7 C8 C7 114.7(3) . . ?
C9 C8 C7 125.0(3) . . ?
N6 C9 C8 122.7(3) . . ?
N6 C10 C11 123.4(4) . . ?
N7 C11 C10 120.8(4) . . ?
O4 C12 O5 125.7(3) . . ?
O4 C12 C13 117.8(3) . . ?
O5 C12 C13 116.5(3) . . ?
N8 C13 C14 123.5(3) . . ?
N8 C13 C12 117.1(3) . . ?
C14 C13 C12 119.5(3) . . ?
C15 C14 C13 118.0(3) . . ?
C14 C15 C16 116.7(3) . . ?
N9 C16 C15 122.4(3) . . ?
N9 C16 C17 114.8(2) . . ?
C15 C16 C17 122.8(3) . . ?
O6 C17 N10 126.6(2) . . ?
O6 C17 C16 117.5(2) . . ?
N10 C17 C16 116.0(2) . . ?
N11 C18 N12 125.2(3) . . ?
N11 C18 C19 112.7(3) . . ?
N12 C18 C19 122.1(3) . . ?
N14 C19 C20 120.3(3) . . ?
N14 C19 C18 114.6(3) . . ?
C20 C19 C18 125.1(3) . . ?
N13 C20 C19 121.8(3) . . ?
N13 C21 C22 121.9(3) . . ?
N14 C22 C21 120.7(3) . . ?
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 N11 1.959(2) . ?
Ni1 N4 1.965(2) . ?
Ni1 N7 2.114(3) . ?
Ni1 O6 2.1212(19) . ?
Ni1 N14 2.124(3) . ?
Ni1 O3 2.129(2) . ?
Ni2 O8 2.066(3) . ?
Ni2 O6 2.0663(19) 2 ?
Ni2 N9 2.071(2) 2 ?
Ni2 O3 2.072(2) . ?
Ni2 N2 2.080(2) . ?
Ni2 O7 2.082(2) . ?
O1 C1 1.245(4) . ?
O2 C1 1.257(4) . ?
O3 C6 1.308(3) . ?
O4 C12 1.241(4) . ?
O5 C12 1.250(4) . ?
O6 C17 1.305(3) . ?
O6 Ni2 2.0663(19) 2 ?
N1 C2 1.331(4) . ?
N1 N2 1.338(4) . ?
N2 C5 1.329(4) . ?
N3 C6 1.305(4) . ?
N3 N4 1.393(3) . ?
N4 C7 1.304(4) . ?
N5 C7 1.326(4) . ?
N6 C9 1.324(5) . ?
N6 C10 1.328(5) . ?
N7 C11 1.337(4) . ?
N7 C8 1.353(4) . ?
N8 C13 1.327(4) . ?
N8 N9 1.342(3) . ?
N9 C16 1.320(4) . ?
N9 Ni2 2.071(2) 2 ?
N10 C17 1.307(4) . ?
N10 N11 1.399(3) . ?
N11 C18 1.295(4) . ?
N12 C18 1.324(4) . ?
N13 C21 1.321(5) . ?
N13 C20 1.337(5) . ?
N14 C22 1.332(4) . ?
N14 C19 1.355(4) . ?
C1 C2 1.522(5) . ?
C2 C3 1.392(4) . ?
C3 C4 1.348(4) . ?
C4 C5 1.401(4) . ?
C5 C6 1.460(4) . ?
C7 C8 1.475(4) . ?
C8 C9 1.385(5) . ?
C10 C11 1.366(6) . ?
C12 C13 1.524(4) . ?
C13 C14 1.400(4) . ?
C14 C15 1.368(4) . ?
C15 C16 1.405(4) . ?
C16 C17 1.479(4) . ?
C18 C19 1.482(4) . ?
C19 C20 1.386(4) . ?
C21 C22 1.397(5) . ?
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
1 0.198 0.044 0.511 2685.4 345.6
