#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005406.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_7005406
loop_
_publ_author_name
'Klingele, Julia'
'Prikhod'ko, Alexander I.'
'Leibeling, Guido'
'Demeshko, Serhiy'
'Dechert, Sebastian'
'Meyer, Franc'
_publ_section_title
;
 Pyrazolate-based copper(II) and nickel(II) [2 x 2] grid complexes:
 protonation-dependent self-assembly, structures and properties.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2003
_journal_page_last               2013
_journal_paper_doi               10.1039/b701981e
_journal_year                    2007
_chemical_formula_moiety         'C68 H56 N24 Ni4 O8, 8(H2 O)'
_chemical_formula_sum            'C68 H72 N24 Ni4 O16'
_chemical_formula_weight         1716.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.7567(9)
_cell_length_b                   22.7567(9)
_cell_length_c                   13.7394(7)
_cell_measurement_reflns_used    53638
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      1.73
_cell_volume                     7115.2(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53638
_diffrn_reflns_theta_full        24.90
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.130
_exptl_absorpt_correction_T_max  0.8819
_exptl_absorpt_correction_T_min  0.7263
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0288
_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)+(0.0395P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                2415
_reflns_number_total             3081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701981e.txt
_cod_data_source_block           Ni4L4
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7005406
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.581870(12) 0.700012(13) 0.537474(19) 0.02043(10) Uani 1 1 d . . .
N1 N 0.50219(8) 0.67911(8) 0.51915(12) 0.0216(4) Uani 1 1 d . . .
N2 N 0.45425(8) 0.66882(8) 0.57489(13) 0.0217(4) Uani 1 1 d . . .
N3 N 0.58401(8) 0.69517(8) 0.40348(13) 0.0244(4) Uani 1 1 d . . .
N4 N 0.66261(8) 0.72118(8) 0.52373(13) 0.0243(4) Uani 1 1 d . . .
N5 N 0.31023(9) 0.62075(10) 0.49448(16) 0.0318(5) Uani 1 1 d . . .
N6 N 0.19530(11) 0.51170(10) 0.53912(17) 0.0453(6) Uani 1 1 d . . .
O1 O 0.53010(7) 0.67407(7) 0.26481(10) 0.0293(4) Uani 1 1 d . . .
O2 O 0.34539(7) 0.63642(8) 0.64632(11) 0.0316(4) Uani 1 1 d . . .
C1 C 0.43003(10) 0.65197(10) 0.41799(16) 0.0240(5) Uani 1 1 d . . .
H1 H 0.4091 0.6422 0.3621 0.080 Uiso 1 1 calc R . .
C2 C 0.48761(10) 0.66931(10) 0.42491(15) 0.0215(5) Uani 1 1 d . . .
C3 C 0.40993(10) 0.65238(10) 0.51417(16) 0.0225(5) Uani 1 1 d . . .
C4 C 0.53623(11) 0.67965(9) 0.35543(15) 0.0242(5) Uani 1 1 d . . .
C5 C 0.63818(10) 0.71051(11) 0.35359(16) 0.0279(5) Uani 1 1 d . . .
H5A H 0.6320 0.7442 0.3116 0.080 Uiso 1 1 calc R . .
H5B H 0.6517 0.6778 0.3142 0.080 Uiso 1 1 calc R . .
C6 C 0.68233(10) 0.72471(10) 0.43091(16) 0.0258(5) Uani 1 1 d . . .
C7 C 0.74007(11) 0.73949(11) 0.40994(18) 0.0320(6) Uani 1 1 d . . .
H7 H 0.7525 0.7422 0.3456 0.080 Uiso 1 1 calc R . .
C8 C 0.77910(11) 0.75010(12) 0.48512(19) 0.0359(6) Uani 1 1 d . . .
H8 H 0.8180 0.7598 0.4722 0.080 Uiso 1 1 calc R . .
C9 C 0.75895(11) 0.74595(12) 0.58013(19) 0.0338(6) Uani 1 1 d . . .
H9 H 0.7843 0.7527 0.6320 0.080 Uiso 1 1 calc R . .
C10 C 0.70117(11) 0.73183(11) 0.59680(18) 0.0298(5) Uani 1 1 d . . .
H10 H 0.6880 0.7295 0.6607 0.080 Uiso 1 1 calc R . .
C11 C 0.35285(10) 0.63632(10) 0.55751(16) 0.0246(5) Uani 1 1 d . . .
C12 C 0.25386(11) 0.59911(11) 0.52773(19) 0.0345(6) Uani 1 1 d . . .
H12A H 0.2236 0.6130 0.4837 0.080 Uiso 1 1 calc R . .
H12B H 0.2458 0.6156 0.5915 0.080 Uiso 1 1 calc R . .
C13 C 0.24997(12) 0.53286(11) 0.53415(17) 0.0334(6) Uani 1 1 d . . .
C14 C 0.29896(15) 0.49642(13) 0.5368(2) 0.0464(7) Uani 1 1 d . . .
H14 H 0.3365 0.5124 0.5329 0.080 Uiso 1 1 calc R . .
C15 C 0.29164(19) 0.43693(15) 0.5452(2) 0.0617(10) Uani 1 1 d . . .
H15 H 0.3240 0.4121 0.5480 0.080 Uiso 1 1 calc R . .
C16 C 0.2358(2) 0.41462(15) 0.5492(2) 0.0664(11) Uani 1 1 d . . .
H16 H 0.2295 0.3743 0.5537 0.080 Uiso 1 1 calc R . .
C17 C 0.18933(18) 0.45291(15) 0.5465(2) 0.0613(10) Uani 1 1 d . . .
H17 H 0.1515 0.4375 0.5498 0.080 Uiso 1 1 calc R . .
O3 O 0.08811(11) 0.56883(11) 0.51134(19) 0.0530(6) Uani 1 1 d . . .
O4 O 0.59434(10) 0.67467(10) 0.09294(16) 0.0447(5) Uani 1 1 d . . .
H3A H 0.1262(18) 0.5514(16) 0.510(3) 0.068(11) Uiso 1 1 d . . .
H3B H 0.0853(15) 0.5945(15) 0.471(2) 0.050(11) Uiso 1 1 d . . .
H4A H 0.5789(17) 0.6809(16) 0.148(3) 0.074(12) Uiso 1 1 d . . .
H4B H 0.5831(14) 0.7031(15) 0.064(3) 0.053(11) Uiso 1 1 d . . .
H5 H 0.3165(13) 0.6233(13) 0.433(2) 0.049(9) Uiso 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
N3 Ni1 N1 82.96(8) . . ?
N3 Ni1 N2 178.85(9) . 12_767 ?
N1 Ni1 N2 97.92(8) . 12_767 ?
N3 Ni1 N4 83.74(8) . . ?
N1 Ni1 N4 166.67(7) . . ?
N2 Ni1 N4 95.39(8) 12_767 . ?
N3 Ni1 O2 106.37(7) . 12_767 ?
N1 Ni1 O2 94.64(7) . 12_767 ?
N2 Ni1 O2 72.85(7) 12_767 12_767 ?
N4 Ni1 O2 89.92(7) . 12_767 ?
N3 Ni1 Ni1 128.49(6) . 15_566 ?
N1 Ni1 Ni1 45.58(5) . 15_566 ?
N2 Ni1 Ni1 52.36(6) 12_767 15_566 ?
N4 Ni1 Ni1 147.74(6) . 15_566 ?
O2 Ni1 Ni1 80.28(4) 12_767 15_566 ?
N3 Ni1 Ni1 93.08(6) . 6_564 ?
N1 Ni1 Ni1 46.59(5) . 6_564 ?
N2 Ni1 Ni1 88.07(6) 12_767 6_564 ?
N4 Ni1 Ni1 133.63(6) . 6_564 ?
O2 Ni1 Ni1 134.50(4) 12_767 6_564 ?
Ni1 Ni1 Ni1 56.096(4) 15_566 6_564 ?
N3 Ni1 Ni1 64.51(6) . 7_544 ?
N1 Ni1 Ni1 68.97(5) . 7_544 ?
N2 Ni1 Ni1 115.08(6) 12_767 7_544 ?
N4 Ni1 Ni1 105.80(6) . 7_544 ?
O2 Ni1 Ni1 47.36(4) 12_767 7_544 ?
Ni1 Ni1 Ni1 90.009(8) 15_566 7_544 ?
Ni1 Ni1 Ni1 114.359(9) 6_564 7_544 ?
N2 N1 C2 108.36(18) . . ?
N2 N1 Ni1 137.81(14) . . ?
C2 N1 Ni1 113.78(15) . . ?
N1 N2 C3 107.33(17) . . ?
N1 N2 Ni1 127.42(14) . 15_566 ?
C3 N2 Ni1 124.89(15) . 15_566 ?
C4 N3 C5 121.81(18) . . ?
C4 N3 Ni1 119.56(15) . . ?
C5 N3 Ni1 118.61(15) . . ?
C6 N4 C10 118.2(2) . . ?
C6 N4 Ni1 115.27(15) . . ?
C10 N4 Ni1 126.52(16) . . ?
C11 N5 C12 121.6(2) . . ?
C13 N6 C17 117.1(3) . . ?
C2 C1 C3 104.19(19) . . ?
N1 C2 C1 110.33(19) . . ?
N1 C2 C4 114.0(2) . . ?
C1 C2 C4 135.6(2) . . ?
N2 C3 C1 109.8(2) . . ?
N2 C3 C11 118.24(19) . . ?
C1 C3 C11 131.9(2) . . ?
O1 C4 N3 127.8(2) . . ?
O1 C4 C2 122.6(2) . . ?
N3 C4 C2 109.61(18) . . ?
N3 C5 C6 106.64(18) . . ?
N4 C6 C7 121.6(2) . . ?
N4 C6 C5 115.7(2) . . ?
C7 C6 C5 122.7(2) . . ?
C8 C7 C6 119.7(2) . . ?
C7 C8 C9 118.6(2) . . ?
C10 C9 C8 119.3(2) . . ?
N4 C10 C9 122.6(2) . . ?
O2 C11 N5 122.5(2) . . ?
O2 C11 C3 121.4(2) . . ?
N5 C11 C3 116.1(2) . . ?
N5 C12 C13 114.2(2) . . ?
N6 C13 C14 122.0(3) . . ?
N6 C13 C12 114.6(2) . . ?
C14 C13 C12 123.3(2) . . ?
C15 C14 C13 119.6(3) . . ?
C14 C15 C16 118.9(3) . . ?
C17 C16 C15 118.6(3) . . ?
N6 C17 C16 123.7(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 N3 1.8450(18) . ?
Ni1 N1 1.8914(19) . ?
Ni1 N2 1.8935(18) 12_767 ?
Ni1 N4 1.909(2) . ?
Ni1 O2 2.6489(16) 12_767 ?
Ni1 Ni1 3.9134(5) 15_566 ?
Ni1 Ni1 4.3658(6) 6_564 ?
Ni1 Ni1 9.0835(5) 7_544 ?
N1 N2 1.353(3) . ?
N1 C2 1.355(3) . ?
N2 C3 1.361(3) . ?
N2 Ni1 1.8935(18) 15_566 ?
N3 C4 1.320(3) . ?
N3 C5 1.453(3) . ?
N4 C6 1.354(3) . ?
N4 C10 1.355(3) . ?
N5 C11 1.348(3) . ?
N5 C12 1.448(3) . ?
N6 C13 1.336(3) . ?
N6 C17 1.348(4) . ?
O1 C4 1.259(3) . ?
O2 C11 1.232(3) . ?
C1 C2 1.372(3) . ?
C1 C3 1.398(3) . ?
C2 C4 1.480(3) . ?
C3 C11 1.475(3) . ?
C5 C6 1.497(3) . ?
C6 C7 1.387(3) . ?
C7 C8 1.384(4) . ?
C8 C9 1.387(4) . ?
C9 C10 1.373(3) . ?
C12 C13 1.513(4) . ?
C13 C14 1.390(4) . ?
C14 C15 1.369(4) . ?
C15 C16 1.370(5) . ?
C16 C17 1.370(5) . ?
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
N5 H5 O3 0.86(3) 2.52(3) 3.343(4) 162(3) 4_454
O3 H3B O4 0.81(3) 2.03(4) 2.806(4) 159(3) 10_556
O3 H3A N6 0.95(4) 1.86(4) 2.790(4) 166(3) .
O4 H4A O1 0.85(4) 1.95(4) 2.777(3) 163(4) .
O4 H4B O1 0.80(4) 2.07(4) 2.850(3) 166(3) 12_766
