#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:11:53 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179618 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/82/4508223.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_4508223
loop_
_publ_author_name
'Moustapha-Sow, Mouhamadou'
'Diouf, Ousmane'
'Gaye, Mohamed'
'Salam-Sall, Abdou'
'Castro, Goretti'
'Pérez-Lourido, Paulo'
'Valencia, Laura'
'Caneschi, Andrea'
'Sorace, Lorenzo'
_publ_section_title
;
 Sheets of Tetranuclear Ni(II) [2 × 2] Square Grids Structure with
 Infinite Orthogonal Two-Dimensional Water--Chlorine Chains
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4172
_journal_paper_doi               10.1021/cg400885f
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C60 H68 Cl4 N24 Ni4 O8'
_chemical_formula_weight         1630.02
_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                   14.164(5)
_cell_length_b                   14.164(5)
_cell_length_c                   34.886(13)
_cell_measurement_temperature    293(2)
_cell_volume                     6999(4)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_data_reduction        'BRUKER Shelxtl'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'BRUKER CCD-1000'
_diffrn_measurement_method       '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  0.1377
_diffrn_reflns_av_sigmaI/netI    0.1301
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            19198
_diffrn_reflns_theta_full        28.16
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.8210
_exptl_absorpt_correction_T_min  0.7151
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.2216
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1603P)²+49.7378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.3380
_reflns_number_gt                1787
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400885f_si_001.cif
_cod_data_source_block           '[Ni4(HL)4]Cl4.4H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6998(5)
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               4508223
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
C1 C 0.3680(7) 0.1894(7) 0.1338(3) 0.058(3) Uani 1 1 d .
H1 H 0.3581 0.2032 0.1595 0.069 Uiso 1 1 calc R
C2 C 0.4452(9) 0.1357(10) 0.1239(4) 0.081(4) Uani 1 1 d .
H2 H 0.4861 0.1125 0.1425 0.097 Uiso 1 1 calc R
C3 C 0.4602(10) 0.1170(10) 0.0851(5) 0.090(4) Uani 1 1 d .
H3 H 0.5124 0.0820 0.0773 0.108 Uiso 1 1 calc R
C4 C 0.3961(8) 0.1512(9) 0.0579(4) 0.068(3) Uani 1 1 d .
H4 H 0.4047 0.1395 0.0319 0.081 Uiso 1 1 calc R
C5 C 0.3217(7) 0.2015(7) 0.0703(3) 0.050(2) Uani 1 1 d .
C6 C 0.2460(7) 0.2362(7) 0.0441(3) 0.048(2) Uani 1 1 d .
C7 C 0.2506(9) 0.2228(9) 0.0010(3) 0.069(3) Uani 1 1 d .
H7A H 0.1892 0.2334 -0.0099 0.104 Uiso 1 1 calc R
H7B H 0.2706 0.1596 -0.0047 0.104 Uiso 1 1 calc R
H7C H 0.2947 0.2668 -0.0098 0.104 Uiso 1 1 calc R
C8 C 0.0417(6) 0.3671(6) 0.0675(3) 0.043(2) Uani 1 1 d .
C9 C 0.2952(7) 0.4795(8) 0.0847(3) 0.059(3) Uani 1 1 d .
H9 H 0.2804 0.4560 0.0605 0.071 Uiso 1 1 calc R
C10 C 0.3482(8) 0.5622(8) 0.0874(4) 0.071(3) Uani 1 1 d .
H10 H 0.3690 0.5933 0.0655 0.085 Uiso 1 1 calc R
C11 C 0.3693(8) 0.5973(8) 0.1239(4) 0.067(3) Uani 1 1 d .
H11 H 0.4053 0.6518 0.1266 0.080 Uiso 1 1 calc R
C12 C 0.3368(8) 0.5509(8) 0.1555(4) 0.063(3) Uani 1 1 d .
H12 H 0.3492 0.5741 0.1799 0.076 Uiso 1 1 calc R
C13 C 0.2849(7) 0.4687(7) 0.1508(3) 0.047(2) Uani 1 1 d .
C14 C 0.2483(7) 0.4119(7) 0.1835(3) 0.049(2) Uani 1 1 d .
C15 C 0.2681(10) 0.4363(9) 0.2243(3) 0.076(4) Uani 1 1 d .
H15A H 0.2482 0.3852 0.2406 0.113 Uiso 1 1 calc R
H15B H 0.2342 0.4925 0.2311 0.113 Uiso 1 1 calc R
H15C H 0.3346 0.4467 0.2276 0.113 Uiso 1 1 calc R
N1 N 0.3072(5) 0.2224(5) 0.1082(3) 0.049(2) Uani 1 1 d .
N2 N 0.1792(5) 0.2789(5) 0.0619(2) 0.0433(18) Uani 1 1 d .
N3 N 0.1035(5) 0.3202(6) 0.0438(2) 0.049(2) Uani 1 1 d .
H3A H 0.0954 0.3170 0.0194 0.059 Uiso 1 1 calc R
N4 N 0.2654(6) 0.4336(5) 0.1152(2) 0.0477(19) Uani 1 1 d .
N5 N 0.1984(5) 0.3386(5) 0.1730(2) 0.0437(18) Uani 1 1 d .
N6 N 0.1586(6) 0.2806(6) 0.1998(2) 0.0480(19) Uani 1 1 d .
O1 O 0.0593(4) 0.3688(4) 0.10373(17) 0.0447(15) Uani 1 1 d .
Ni1 Ni 0.18972(8) 0.30563(8) 0.11782(3) 0.0429(4) Uani 1 1 d .
Cl1 Cl 0.0000 0.2500 0.96889(16) 0.177(5) Uani 1 2 d S
Cl2 Cl 0.5000 0.7500 0.0518(2) 0.143(3) Uani 1 2 d S
O1W O 0.5738(5) 0.0778(4) 0.99571(18) 0.0493(17) 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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C2 122.8(11) . .
N1 C1 H1 118.6 . .
C2 C1 H1 118.6 . .
C1 C2 C3 118.0(11) . .
C1 C2 H2 121.0 . .
C3 C2 H2 121.0 . .
C2 C3 C4 119.5(12) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C5 C4 C3 118.4(12) . .
C5 C4 H4 120.8 . .
C3 C4 H4 120.8 . .
C4 C5 N1 122.8(10) . .
C4 C5 C6 122.8(10) . .
N1 C5 C6 114.3(8) . .
N2 C6 C5 112.9(9) . .
N2 C6 C7 124.8(9) . .
C5 C6 C7 122.3(8) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O1 C8 N6 126.0(8) . 12_666
O1 C8 N3 118.4(8) . .
N6 C8 N3 115.6(8) 12_666 .
N4 C9 C10 122.1(11) . .
N4 C9 H9 118.9 . .
C10 C9 H9 118.9 . .
C9 C10 C11 118.5(11) . .
C9 C10 H10 120.8 . .
C11 C10 H10 120.8 . .
C12 C11 C10 119.5(10) . .
C12 C11 H11 120.3 . .
C10 C11 H11 120.3 . .
C11 C12 C13 119.2(11) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
N4 C13 C12 121.4(10) . .
N4 C13 C14 115.5(8) . .
C12 C13 C14 123.1(10) . .
N5 C14 C13 113.6(9) . .
N5 C14 C15 123.5(9) . .
C13 C14 C15 122.8(9) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C1 N1 C5 118.4(9) . .
C1 N1 Ni1 127.9(8) . .
C5 N1 Ni1 113.6(6) . .
C6 N2 N3 123.6(8) . .
C6 N2 Ni1 120.6(7) . .
N3 N2 Ni1 115.3(6) . .
N2 N3 C8 115.2(7) . .
N2 N3 H3A 122.4 . .
C8 N3 H3A 122.4 . .
C9 N4 C13 119.3(9) . .
C9 N4 Ni1 128.5(7) . .
C13 N4 Ni1 112.1(6) . .
C14 N5 N6 120.6(8) . .
C14 N5 Ni1 119.5(7) . .
N6 N5 Ni1 119.7(6) . .
C8 N6 N5 109.7(7) 15 .
C8 O1 Ni1 113.0(6) . .
C8 O1 Ni1 108.3(5) . 12_666
Ni1 O1 Ni1 138.7(3) . 12_666
N5 Ni1 N2 177.3(3) . .
N5 Ni1 N1 104.0(3) . .
N2 Ni1 N1 78.0(3) . .
N5 Ni1 N4 79.0(3) . .
N2 Ni1 N4 99.1(3) . .
N1 Ni1 N4 94.2(3) . .
N5 Ni1 O1 100.4(3) . .
N2 Ni1 O1 77.7(3) . .
N1 Ni1 O1 155.3(3) . .
N4 Ni1 O1 94.1(3) . .
N5 Ni1 O1 76.1(3) . 15
N2 Ni1 O1 105.8(3) . 15
N1 Ni1 O1 91.1(3) . 15
N4 Ni1 O1 155.1(3) . 15
O1 Ni1 O1 91.1(3) . 15
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.326(12) .
C1 C2 1.376(16) .
C1 H1 0.9300 .
C2 C3 1.396(18) .
C2 H2 0.9300 .
C3 C4 1.399(18) .
C3 H3 0.9300 .
C4 C5 1.342(14) .
C4 H4 0.9300 .
C5 N1 1.371(13) .
C5 C6 1.493(14) .
C6 N2 1.282(11) .
C6 C7 1.517(14) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 O1 1.288(10) .
C8 N6 1.324(11) 12_666
C8 N3 1.377(12) .
C9 N4 1.316(13) .
C9 C10 1.395(16) .
C9 H9 0.9300 .
C10 C11 1.398(17) .
C10 H10 0.9300 .
C11 C12 1.363(16) .
C11 H11 0.9300 .
C12 C13 1.386(14) .
C12 H12 0.9300 .
C13 N4 1.366(12) .
C13 C14 1.490(14) .
C14 N5 1.308(12) .
C14 C15 1.491(15) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
N1 Ni1 2.067(8) .
N2 N3 1.375(10) .
N2 Ni1 1.994(8) .
N3 H3A 0.8600 .
N4 Ni1 2.107(8) .
N5 N6 1.366(11) .
N5 Ni1 1.986(8) .
N6 C8 1.324(12) 15
O1 Ni1 2.110(6) .
O1 Ni1 2.155(6) 12_666
Ni1 O1 2.155(6) 15
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
N1 C1 C2 C3 1(2) . .
C1 C2 C3 C4 -1(2) . .
C2 C3 C4 C5 0(2) . .
C3 C4 C5 N1 1.6(18) . .
C3 C4 C5 C6 -176.1(11) . .
C4 C5 C6 N2 177.0(10) . .
N1 C5 C6 N2 -0.9(12) . .
C4 C5 C6 C7 -4.1(16) . .
N1 C5 C6 C7 178.0(9) . .
N4 C9 C10 C11 -0.5(17) . .
C9 C10 C11 C12 -0.9(18) . .
C10 C11 C12 C13 1.3(18) . .
C11 C12 C13 N4 -0.2(16) . .
C11 C12 C13 C14 178.5(10) . .
N4 C13 C14 N5 -3.3(12) . .
C12 C13 C14 N5 177.9(9) . .
N4 C13 C14 C15 176.0(10) . .
C12 C13 C14 C15 -2.8(16) . .
C2 C1 N1 C5 0.4(16) . .
C2 C1 N1 Ni1 -178.8(9) . .
C4 C5 N1 C1 -1.9(15) . .
C6 C5 N1 C1 176.0(9) . .
C4 C5 N1 Ni1 177.5(9) . .
C6 C5 N1 Ni1 -4.6(10) . .
C5 C6 N2 N3 177.4(8) . .
C7 C6 N2 N3 -1.6(15) . .
C5 C6 N2 Ni1 6.6(11) . .
C7 C6 N2 Ni1 -172.3(8) . .
C6 N2 N3 C8 -176.6(9) . .
Ni1 N2 N3 C8 -5.4(10) . .
O1 C8 N3 N2 0.2(12) . .
N6 C8 N3 N2 178.8(8) 12_666 .
C10 C9 N4 C13 1.6(15) . .
C10 C9 N4 Ni1 -177.4(8) . .
C12 C13 N4 C9 -1.2(14) . .
C14 C13 N4 C9 180.0(9) . .
C12 C13 N4 Ni1 177.9(8) . .
C14 C13 N4 Ni1 -0.9(10) . .
C13 C14 N5 N6 -178.8(8) . .
C15 C14 N5 N6 1.9(15) . .
C13 C14 N5 Ni1 6.3(11) . .
C15 C14 N5 Ni1 -172.9(9) . .
C14 N5 N6 C8 -175.9(9) . 15
Ni1 N5 N6 C8 -1.1(10) . 15
N6 C8 O1 Ni1 -173.7(8) 12_666 .
N3 C8 O1 Ni1 4.7(10) . .
N6 C8 O1 Ni1 5.1(11) 12_666 12_666
N3 C8 O1 Ni1 -176.4(7) . 12_666
C14 N5 Ni1 N2 -51(7) . .
N6 N5 Ni1 N2 134(6) . .
C14 N5 Ni1 N1 86.2(8) . .
N6 N5 Ni1 N1 -88.7(7) . .
C14 N5 Ni1 N4 -5.4(7) . .
N6 N5 Ni1 N4 179.7(7) . .
C14 N5 Ni1 O1 -97.6(7) . .
N6 N5 Ni1 O1 87.5(7) . .
C14 N5 Ni1 O1 173.9(8) . 15
N6 N5 Ni1 O1 -1.0(6) . 15
C6 N2 Ni1 N5 130(6) . .
N3 N2 Ni1 N5 -41(7) . .
C6 N2 Ni1 N1 -7.3(7) . .
N3 N2 Ni1 N1 -178.7(7) . .
C6 N2 Ni1 N4 85.2(8) . .
N3 N2 Ni1 N4 -86.3(6) . .
C6 N2 Ni1 O1 177.4(8) . .
N3 N2 Ni1 O1 5.9(6) . .
C6 N2 Ni1 O1 -95.0(8) . 15
N3 N2 Ni1 O1 93.5(6) . 15
C1 N1 Ni1 N5 7.2(9) . .
C5 N1 Ni1 N5 -172.1(6) . .
C1 N1 Ni1 N2 -174.7(9) . .
C5 N1 Ni1 N2 6.0(6) . .
C1 N1 Ni1 N4 86.9(9) . .
C5 N1 Ni1 N4 -92.4(7) . .
C1 N1 Ni1 O1 -163.8(7) . .
C5 N1 Ni1 O1 16.9(11) . .
C1 N1 Ni1 O1 -68.7(8) . 15
C5 N1 Ni1 O1 112.0(6) . 15
C9 N4 Ni1 N5 -177.9(9) . .
C13 N4 Ni1 N5 3.1(6) . .
C9 N4 Ni1 N2 0.1(9) . .
C13 N4 Ni1 N2 -178.9(6) . .
C9 N4 Ni1 N1 78.7(9) . .
C13 N4 Ni1 N1 -100.3(6) . .
C9 N4 Ni1 O1 -78.0(9) . .
C13 N4 Ni1 O1 103.0(6) . .
C9 N4 Ni1 O1 -179.5(7) . 15
C13 N4 Ni1 O1 1.5(11) . 15
C8 O1 Ni1 N5 172.2(6) . .
Ni1 O1 Ni1 N5 -6.2(5) 12_666 .
C8 O1 Ni1 N2 -5.7(6) . .
Ni1 O1 Ni1 N2 175.9(5) 12_666 .
C8 O1 Ni1 N1 -16.6(10) . .
Ni1 O1 Ni1 N1 165.0(5) 12_666 .
C8 O1 Ni1 N4 92.7(6) . .
Ni1 O1 Ni1 N4 -85.7(5) 12_666 .
C8 O1 Ni1 O1 -111.7(6) . 15
Ni1 O1 Ni1 O1 69.9(5) 12_666 15
