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#$Date: 2016-03-26 20:54:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180454 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/23/7212357.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_7212357
loop_
_publ_author_name
'McMurtrie, John'
'Dance, Ian'
_publ_section_title
;
 Alternative metal grid structures formed by [M(terpy)2]2+ and
 [M(terpyOH)2]2+ complexes with small and large tetrahedral dianions, and
 by [Ru(terpy)2]0
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2700
_journal_paper_doi               10.1039/b926074a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C30 H22 N6 Ni1, 1(S O4), 4(C3 H8 O)'
_chemical_formula_sum            'C42 H54 N6 Ni O8 S'
_chemical_formula_weight         861.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                   9.0281(4)
_cell_length_b                   9.0281(4)
_cell_length_c                   24.6380(17)
_cell_measurement_reflns_used    3403
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.2865
_cell_measurement_theta_min      2.398
_cell_volume                     2008.16(19)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 1995)'
_computing_molecular_graphics
;ORTEPIII (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.0 (CCDC, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Brucker SMART 1000 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22055
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.08
_diffrn_standards_number         120
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.8067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0670
_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)+(0.0500P)²+7.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                1983
_reflns_number_total             2457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926074a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               7212357
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Ni1 Ni 0.5000 0.0000 0.2500 0.0400(3) Uani 1 4 d S
S1 S 0.0000 0.0000 0.5000 0.0711(10) Uani 1 4 d SU
O1 O 0.0224(9) 0.1239(9) 0.4665(3) 0.138(3) Uani 1 1 d U
N1 N 0.2912(5) 0.0917(4) 0.26700(15) 0.0424(10) Uani 1 1 d .
N2 N 0.5000 0.0000 0.33063(19) 0.0456(12) Uani 1 2 d S
C1 C 0.1880(6) 0.1398(6) 0.2321(2) 0.0524(14) Uani 1 1 d .
H1A H 0.2093 0.1351 0.1944 0.063 Uiso 1 1 calc R
C2 C 0.0526(5) 0.1957(6) 0.2479(4) 0.0603(13) Uani 1 1 d .
H2A H -0.0174 0.2283 0.2217 0.072 Uiso 1 1 calc R
C3 C 0.0211(7) 0.2031(7) 0.3020(3) 0.0641(17) Uani 1 1 d .
H3A H -0.0706 0.2427 0.3141 0.077 Uiso 1 1 calc R
C4 C 0.1250(7) 0.1521(7) 0.3392(3) 0.0624(16) Uani 1 1 d .
H4A H 0.1041 0.1530 0.3770 0.075 Uiso 1 1 calc R
C5 C 0.2582(6) 0.1004(6) 0.3203(2) 0.0498(12) Uani 1 1 d .
C6 C 0.3801(7) 0.0492(7) 0.3569(2) 0.0593(16) Uani 1 1 d .
C7 C 0.3762(10) 0.0494(10) 0.4136(3) 0.098(3) Uani 1 1 d U
H7A H 0.2911 0.0825 0.4328 0.117 Uiso 1 1 calc R
C8 C 0.5000 0.0000 0.4406(4) 0.114(4) Uani 1 2 d SU
H8A H 0.5000 0.0000 0.4791 0.137 Uiso 1 2 calc SR
O2 O 0.2578(10) 0.2964(9) 0.1007(3) 0.152(3) Uani 1 1 d DU
H2B H 0.2964 0.3692 0.0849 0.182 Uiso 1 1 calc R
C9 C 0.2121(19) 0.203(2) 0.0654(7) 0.213(8) Uani 1 1 d DU
H9A H 0.2164 0.1019 0.0810 0.255 Uiso 1 1 calc R
H9B H 0.2786 0.2054 0.0334 0.255 Uiso 1 1 calc R
C10 C 0.060(2) 0.234(3) 0.0479(7) 0.247(10) Uani 1 1 d DU
H10A H 0.0210 0.1467 0.0285 0.296 Uiso 1 1 calc R
H10B H 0.0621 0.3181 0.0221 0.296 Uiso 1 1 calc R
C11 C -0.040(2) 0.271(3) 0.0931(9) 0.267(10) Uani 1 1 d DU
H11A H 0.0173 0.3148 0.1229 0.400 Uiso 1 1 calc R
H11B H -0.0888 0.1806 0.1059 0.400 Uiso 1 1 calc R
H11C H -0.1146 0.3418 0.0806 0.400 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'
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
N2 Ni1 N2 180.0 . 7
N2 Ni1 N1 101.50(10) . 8_545
N2 Ni1 N1 78.50(10) 7 8_545
N2 Ni1 N1 78.50(10) . 2_655
N2 Ni1 N1 101.50(10) 7 2_655
N1 Ni1 N1 92.28(4) 8_545 2_655
N2 Ni1 N1 78.50(10) . .
N2 Ni1 N1 101.50(10) 7 .
N1 Ni1 N1 92.28(4) 8_545 .
N1 Ni1 N1 157.0(2) 2_655 .
N2 Ni1 N1 101.50(10) . 7
N2 Ni1 N1 78.50(10) 7 7
N1 Ni1 N1 157.0(2) 8_545 7
N1 Ni1 N1 92.28(4) 2_655 7
N1 Ni1 N1 92.28(4) . 7
O1 S1 O1 108.0(7) 4_556 3_556
O1 S1 O1 110.2(4) 4_556 2
O1 S1 O1 110.2(3) 3_556 2
O1 S1 O1 110.2(3) 4_556 .
O1 S1 O1 110.2(4) 3_556 .
O1 S1 O1 108.0(7) 2 .
C1 N1 C5 116.9(5) . .
C1 N1 Ni1 128.6(3) . .
C5 N1 Ni1 114.5(3) . .
C6 N2 C6 122.1(6) . 2_655
C6 N2 Ni1 119.0(3) . .
C6 N2 Ni1 119.0(3) 2_655 .
N1 C1 C2 123.6(6) . .
N1 C1 H1A 118.2 . .
C2 C1 H1A 118.2 . .
C3 C2 C1 118.7(7) . .
C3 C2 H2A 120.7 . .
C1 C2 H2A 120.7 . .
C2 C3 C4 119.1(6) . .
C2 C3 H3A 120.4 . .
C4 C3 H3A 120.4 . .
C5 C4 C3 118.8(6) . .
C5 C4 H4A 120.6 . .
C3 C4 H4A 120.6 . .
N1 C5 C4 122.9(5) . .
N1 C5 C6 114.0(5) . .
C4 C5 C6 123.1(5) . .
N2 C6 C7 120.3(5) . .
N2 C6 C5 114.0(4) . .
C7 C6 C5 125.7(5) . .
C8 C7 C6 117.5(7) . .
C8 C7 H7A 121.2 . .
C6 C7 H7A 121.2 . .
C7 C8 C7 122.2(9) 2_655 .
C7 C8 H8A 118.9 2_655 .
C7 C8 H8A 118.9 . .
C9 O2 H2B 109.5 . .
O2 C9 C10 111.8(14) . .
O2 C9 H9A 109.2 . .
C10 C9 H9A 109.2 . .
O2 C9 H9B 109.2 . .
C10 C9 H9B 109.2 . .
H9A C9 H9B 107.9 . .
C9 C10 C11 113.4(14) . .
C9 C10 H10A 108.9 . .
C11 C10 H10A 108.9 . .
C9 C10 H10B 108.9 . .
C11 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N2 1.987(5) .
Ni1 N2 1.987(5) 7
Ni1 N1 2.101(4) 8_545
Ni1 N1 2.101(4) 2_655
Ni1 N1 2.101(4) .
Ni1 N1 2.101(4) 7
S1 O1 1.405(7) 4_556
S1 O1 1.405(7) 3_556
S1 O1 1.405(7) 2
S1 O1 1.405(7) .
N1 C1 1.340(6) .
N1 C5 1.349(6) .
N2 C6 1.337(6) .
N2 C6 1.337(6) 2_655
C1 C2 1.379(8) .
C1 H1A 0.9500 .
C2 C3 1.363(12) .
C2 H2A 0.9500 .
C3 C4 1.390(9) .
C3 H3A 0.9500 .
C4 C5 1.371(8) .
C4 H4A 0.9500 .
C5 C6 1.496(8) .
C6 C7 1.397(9) .
C7 C8 1.375(8) .
C7 H7A 0.9500 .
C8 C7 1.375(8) 2_655
C8 H8A 0.9500 .
O2 C9 1.282(14) .
O2 H2B 0.8400 .
C9 C10 1.463(15) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.472(16) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
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
O2 H2B O1 0.84 2.01 2.836(12) 168.6 8
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
N2 Ni1 N1 C1 178.8(4) . .
N2 Ni1 N1 C1 -1.2(4) 7 .
N1 Ni1 N1 C1 -79.9(5) 8_545 .
N1 Ni1 N1 C1 178.8(4) 2_655 .
N1 Ni1 N1 C1 77.5(4) 7 .
N2 Ni1 N1 C5 -2.3(4) . .
N2 Ni1 N1 C5 177.7(4) 7 .
N1 Ni1 N1 C5 99.0(4) 8_545 .
N1 Ni1 N1 C5 -2.3(4) 2_655 .
N1 Ni1 N1 C5 -103.5(4) 7 .
N2 Ni1 N2 C6 -22(100) 7 .
N1 Ni1 N2 C6 -88.6(4) 8_545 .
N1 Ni1 N2 C6 -178.6(4) 2_655 .
N1 Ni1 N2 C6 1.4(4) . .
N1 Ni1 N2 C6 91.4(4) 7 .
N2 Ni1 N2 C6 158(100) 7 2_655
N1 Ni1 N2 C6 91.4(4) 8_545 2_655
N1 Ni1 N2 C6 1.4(4) 2_655 2_655
N1 Ni1 N2 C6 -178.6(4) . 2_655
N1 Ni1 N2 C6 -88.6(4) 7 2_655
C5 N1 C1 C2 -0.3(7) . .
Ni1 N1 C1 C2 178.6(4) . .
N1 C1 C2 C3 0.1(8) . .
C1 C2 C3 C4 -1.1(9) . .
C2 C3 C4 C5 2.2(10) . .
C1 N1 C5 C4 1.5(8) . .
Ni1 N1 C5 C4 -177.6(5) . .
C1 N1 C5 C6 -178.2(5) . .
Ni1 N1 C5 C6 2.7(6) . .
C3 C4 C5 N1 -2.5(10) . .
C3 C4 C5 C6 177.3(6) . .
C6 N2 C6 C7 -0.5(6) 2_655 .
Ni1 N2 C6 C7 179.5(6) . .
C6 N2 C6 C5 179.6(6) 2_655 .
Ni1 N2 C6 C5 -0.4(6) . .
N1 C5 C6 N2 -1.6(8) . .
C4 C5 C6 N2 178.7(6) . .
N1 C5 C6 C7 178.6(7) . .
C4 C5 C6 C7 -1.2(11) . .
N2 C6 C7 C8 1.1(12) . .
C5 C6 C7 C8 -179.1(6) . .
C6 C7 C8 C7 -0.5(6) . 2_655
O2 C9 C10 C11 -44(3) . .
