#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:12:40 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102681.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_7102681
loop_
_publ_author_name
'Turner, David R'
'Hursthouse, M B'
'Light, M E'
'Steed, Jonathan W'
_publ_section_title
;
 Linear distortion of octahedral metal centres by multiple hydrogen
 bonds in modular ML(4) systems.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1354
_journal_page_last               1355
_journal_paper_doi               10.1039/b402884h
_journal_year                    2004
_chemical_formula_sum            'C52 H58 N12 Ni O12 S'
_chemical_formula_weight         1133.87
_chemical_name_common            '[Ni(TUP)4(H2O)2]SO4.2H2O'
_chemical_name_systematic
;
[Ni(TUP)4(H2O)2]SO4.2H2O
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :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            2
_cell_length_a                   18.028(3)
_cell_length_b                   18.028(3)
_cell_length_c                   8.1143(16)
_cell_measurement_temperature    120(2)
_cell_volume                     2637.3(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.71
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4131
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green/blue
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0121(11)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          1.898
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0396P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                1738
_reflns_number_total             2540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402884h.txt
_cod_data_source_block           C:\Dave\Structs\TUPNiSO4\DTNi021\DTNI021.CIF
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7102681
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-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 0.7500 0.7500 0.24189(7) 0.0181(2) Uani 1 4 d S . .
S1 S 0.7500 1.2500 0.5000 0.0214(3) Uani 1 4 d S . .
N2 N 0.77587(10) 1.03467(9) 0.4842(2) 0.0261(5) Uani 1 1 d . A .
H2N H 0.7753 1.0824 0.4613 0.031 Uiso 1 1 calc R . .
C5 C 0.76169(12) 0.91041(11) 0.3565(3) 0.0222(5) Uani 1 1 d . . .
H5 H 0.7920 0.8888 0.4394 0.027 Uiso 1 1 calc R . .
C8 C 0.83779(12) 1.13245(11) 0.9943(3) 0.0264(6) Uani 1 1 d . . .
H8 H 0.8090 1.1728 0.9547 0.032 Uiso 1 1 calc R . .
N1 N 0.73260(9) 0.86649(9) 0.2403(2) 0.0199(4) Uani 1 1 d . . .
C3 C 0.70980(13) 1.01794(12) 0.2326(3) 0.0285(6) Uani 1 1 d . . .
H3 H 0.7027 1.0701 0.2282 0.034 Uiso 1 1 calc R . .
N3 N 0.81998(10) 1.07297(10) 0.7330(2) 0.0258(5) Uani 1 1 d . A .
H3N H 0.8133 1.1174 0.6907 0.031 Uiso 1 1 calc R . .
C1 C 0.69168(12) 0.89783(12) 0.1219(3) 0.0279(6) Uani 1 1 d . . .
H1 H 0.6692 0.8667 0.0416 0.033 Uiso 1 1 calc R . .
C9 C 0.86886(13) 1.13626(13) 1.1492(3) 0.0293(6) Uani 1 1 d . . .
H9 H 0.8613 1.1794 1.2141 0.035 Uiso 1 1 calc R . .
C2 C 0.68068(13) 0.97309(12) 0.1114(3) 0.0324(6) Uani 1 1 d . . .
H2 H 0.6535 0.9938 0.0222 0.039 Uiso 1 1 calc R . .
C10 C 0.91105(13) 1.07815(13) 1.2126(3) 0.0298(6) Uani 1 1 d . . .
O3A O 0.7938(3) 0.9513(5) 0.6875(14) 0.0309(16) Uani 0.50 1 d P A 1
C11 C 0.91804(14) 1.01574(13) 1.1155(3) 0.0358(7) Uani 1 1 d . . .
H11 H 0.9446 0.9744 1.1578 0.043 Uiso 1 1 calc R . .
C4 C 0.74927(11) 0.98659(11) 0.3606(3) 0.0220(5) Uani 1 1 d . . .
C7 C 0.84789(12) 1.07052(12) 0.8953(3) 0.0247(6) Uani 1 1 d . . .
C6 C 0.80226(14) 1.01512(13) 0.6349(3) 0.0324(6) Uani 1 1 d . . .
C13 C 0.94877(15) 1.08358(16) 1.3767(3) 0.0460(7) Uani 1 1 d . . .
H13A H 0.9483 1.0349 1.4305 0.069 Uiso 1 1 calc R . .
H13C H 0.9225 1.1195 1.4460 0.069 Uiso 1 1 calc R . .
H13B H 1.0002 1.0999 1.3611 0.069 Uiso 1 1 calc R . .
C12 C 0.88804(13) 1.01083(13) 0.9588(3) 0.0347(7) Uani 1 1 d . . .
H12 H 0.8947 0.9671 0.8951 0.042 Uiso 1 1 calc R . .
O4 O 0.68993(8) 1.28093(8) 0.6018(2) 0.0377(5) Uani 1 1 d . . .
O1 O 0.7500 0.7500 0.4979(5) 0.0260(9) Uani 1 4 d S . .
O2 O 0.7500 0.7500 -0.0195(5) 0.0242(8) Uani 1 4 d S . .
O5 O 0.8406(2) 0.8055(2) 0.7357(4) 0.0278(8) Uani 0.50 1 d PD . .
H3O H 0.727(5) 0.777(5) -0.080(8) 0.00(2) Uiso 0.25 1 d P . .
H2O H 0.723(5) 0.726(5) 0.529(10) 0.00(2) Uiso 0.25 1 d P . .
O3B O 0.8250(4) 0.9497(5) 0.6671(14) 0.044(2) Uani 0.50 1 d P A 2
H4O H 0.879(3) 0.788(3) 0.719(6) 0.030(17) Uiso 0.50 1 d PD . .
H5O H 0.853(2) 0.851(3) 0.724(6) 0.020(13) Uiso 0.50 1 d PD . .
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'
S S 0.1246 0.1234 '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
O1 Ni1 O2 180.000(1) . .
O1 Ni1 N1 90.35(5) . 2_655
O2 Ni1 N1 89.65(5) . 2_655
O1 Ni1 N1 90.35(5) . .
O2 Ni1 N1 89.65(5) . .
N1 Ni1 N1 89.998(1) 2_655 .
O1 Ni1 N1 90.35(5) . 3_665
O2 Ni1 N1 89.65(5) . 3_665
N1 Ni1 N1 89.998(1) 2_655 3_665
N1 Ni1 N1 179.31(11) . 3_665
O1 Ni1 N1 90.35(5) . 4_565
O2 Ni1 N1 89.65(5) . 4_565
N1 Ni1 N1 179.31(11) 2_655 4_565
N1 Ni1 N1 89.998(1) . 4_565
N1 Ni1 N1 89.998(1) 3_665 4_565
O4 S1 O4 108.37(7) 8_766 3_675
O4 S1 O4 108.37(7) 8_766 .
O4 S1 O4 111.69(14) 3_675 .
O4 S1 O4 111.69(14) 8_766 6_576
O4 S1 O4 108.37(7) 3_675 6_576
O4 S1 O4 108.37(7) . 6_576
C6 N2 C4 126.87(18) . .
N1 C5 C4 122.5(2) . .
C9 C8 C7 121.0(2) . .
C1 N1 C5 118.19(19) . .
C1 N1 Ni1 120.27(15) . .
C5 N1 Ni1 121.54(14) . .
C2 C3 C4 119.6(2) . .
C6 N3 C7 127.6(2) . .
N1 C1 C2 122.8(2) . .
C8 C9 C10 121.4(2) . .
C1 C2 C3 118.7(2) . .
C11 C10 C9 116.9(2) . .
C11 C10 C13 121.3(2) . .
C9 C10 C13 121.8(2) . .
C10 C11 C12 122.8(2) . .
C3 C4 C5 118.0(2) . .
C3 C4 N2 117.32(19) . .
C5 C4 N2 124.7(2) . .
C8 C7 C12 118.3(2) . .
C8 C7 N3 118.0(2) . .
C12 C7 N3 123.7(2) . .
O3A C6 O3B 27.0(4) . .
O3A C6 N3 123.0(6) . .
O3B C6 N3 121.1(5) . .
O3A C6 N2 120.6(5) . .
O3B C6 N2 122.5(6) . .
N3 C6 N2 114.4(2) . .
C11 C12 C7 119.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.077(4) .
Ni1 O2 2.121(4) .
Ni1 N1 2.1234(17) 2_655
Ni1 N1 2.1234(17) .
Ni1 N1 2.1234(17) 3_665
Ni1 N1 2.1234(17) 4_565
S1 O4 1.4720(15) 8_766
S1 O4 1.4720(15) 3_675
S1 O4 1.4720(15) .
S1 O4 1.4720(15) 6_576
N2 C6 1.359(3) .
N2 C4 1.410(3) .
C5 N1 1.338(3) .
C5 C4 1.392(3) .
C8 C9 1.377(3) .
C8 C7 1.388(3) .
N1 C1 1.336(3) .
C3 C2 1.377(3) .
C3 C4 1.380(3) .
N3 C6 1.350(3) .
N3 C7 1.410(3) .
C1 C2 1.374(3) .
C9 C10 1.393(3) .
C10 C11 1.379(3) .
C10 C13 1.499(3) .
O3A C6 1.237(10) .
C11 C12 1.384(4) .
C7 C12 1.396(3) .
C6 O3B 1.277(10) .
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
N2 H2N O4 0.88 2.25 3.061(2) 153.7 8_766
N3 H3N O4 0.88 1.97 2.846(2) 173.7 3_675
O2 H3O O5 0.80(6) 1.98(6) 2.759(5) 165(8) 2_654
O1 H2O O5 0.70(6) 2.11(7) 2.719(4) 147(9) 3_665
O5 H4O O3A 0.77(5) 1.99(5) 2.709(10) 156(5) 4_565
O5 H4O O3B 0.77(5) 2.45(5) 3.117(10) 147(5) 4_565
O5 H5O O3B 0.87(5) 1.90(5) 2.672(11) 148(4) .
O5 H5O O3A 0.87(5) 2.12(5) 2.788(10) 134(4) .
