#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:47:22 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179815 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/11/7011125.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_7011125
loop_
_publ_author_name
'Harry Adams'
'Scott Clunas'
'David E. Fenton'
'Sharon E. Spey'
_publ_section_title
;
 The systematic generation of monodentate bridging ethanoates in
 dinuclear nickel(II) complexes of asymmetric compartmental ligands
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              441
_journal_page_last               448
_journal_paper_doi               10.1039/b107928j
_journal_year                    2002
_chemical_formula_sum            'C26 H35 N6 Ni2 O4 S2'
_chemical_formula_weight         677.14
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.940(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0082(9)
_cell_length_b                   17.3828(16)
_cell_length_c                   17.2816(16)
_cell_measurement_temperature    150(2)
_cell_volume                     2977.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.1902
_diffrn_reflns_av_sigmaI/netI    0.1419
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18566
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.447
_exptl_absorpt_correction_T_max  0.8559
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0574
_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)+(0.1019P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                5054
_reflns_number_total             7163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107928j.txt
_cod_data_source_block           ifn192m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               7011125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.12124(5) 1.05864(2) 0.70818(3) 0.02001(14) Uani 1 1 d . . .
Ni2 Ni -0.09722(5) 0.95892(2) 0.77111(3) 0.01947(14) Uani 1 1 d . . .
S1 S -0.28424(12) 1.13275(6) 0.57276(7) 0.0396(3) Uani 1 1 d . . .
S2 S -0.24126(13) 1.20191(5) 0.82522(6) 0.0390(3) Uani 1 1 d . . .
O1 O 0.0913(2) 1.00456(12) 0.80766(13) 0.0201(5) Uani 1 1 d . . .
O2 O 0.1473(3) 0.95530(13) 0.65433(16) 0.0256(6) Uani 1 1 d . . .
O3 O -0.0143(3) 0.88725(13) 0.70217(15) 0.0252(6) Uani 1 1 d . . .
O4 O 0.0795(3) 1.16581(13) 0.77302(15) 0.0284(6) Uani 1 1 d . . .
H4 H 0.0320 1.2078 0.7469 0.043 Uiso 1 1 calc R . .
N1 N 0.3185(3) 1.06929(16) 0.74419(18) 0.0245(7) Uani 1 1 d . . .
N2 N 0.1731(3) 1.11762(17) 0.60612(18) 0.0272(7) Uani 1 1 d . . .
N3 N -0.2809(3) 0.91249(16) 0.71946(17) 0.0224(6) Uani 1 1 d . . .
N4 N -0.0839(3) 0.88351(16) 0.86602(17) 0.0219(6) Uani 1 1 d . . .
N5 N -0.1912(3) 1.04372(17) 0.82470(19) 0.0276(7) Uani 1 1 d . . .
N6 N -0.0840(3) 1.05776(17) 0.67428(19) 0.0277(7) Uani 1 1 d . . .
C1 C 0.1880(4) 0.97262(17) 0.8584(2) 0.0207(7) Uani 1 1 d . . .
C2 C 0.1510(4) 0.92757(18) 0.9199(2) 0.0218(7) Uani 1 1 d . . .
C3 C 0.2493(4) 0.89194(19) 0.9734(2) 0.0256(8) Uani 1 1 d . . .
H3A H 0.2216 0.8609 1.0136 0.031 Uiso 1 1 calc R . .
C4 C 0.3876(4) 0.90060(19) 0.9696(2) 0.0264(8) Uani 1 1 d . . .
C5 C 0.4222(4) 0.94738(19) 0.9126(2) 0.0245(8) Uani 1 1 d . . .
H5A H 0.5154 0.9566 0.9111 0.029 Uiso 1 1 calc R . .
C6 C 0.3281(4) 0.98313(18) 0.8554(2) 0.0218(7) Uani 1 1 d . . .
C7 C 0.3856(4) 1.03131(19) 0.8005(2) 0.0235(8) Uani 1 1 d . . .
H7A H 0.4811 1.0353 0.8065 0.028 Uiso 1 1 calc R . .
C8 C 0.3912(4) 1.1166(2) 0.6940(2) 0.0334(9) Uani 1 1 d . . .
H8A H 0.4867 1.1003 0.6983 0.040 Uiso 1 1 calc R . .
H8B H 0.3884 1.1714 0.7093 0.040 Uiso 1 1 calc R . .
C9 C 0.3209(4) 1.1054(2) 0.6107(2) 0.0318(9) Uani 1 1 d . . .
H9A H 0.3582 1.1422 0.5756 0.038 Uiso 1 1 calc R . .
H9B H 0.3384 1.0527 0.5929 0.038 Uiso 1 1 calc R . .
C10 C -0.3182(4) 0.9325(2) 0.6441(2) 0.0278(8) Uani 1 1 d . . .
H10A H -0.2521 0.9550 0.6166 0.033 Uiso 1 1 calc R . .
C11 C -0.4457(4) 0.9224(2) 0.6049(2) 0.0326(9) Uani 1 1 d . . .
H11A H -0.4672 0.9369 0.5516 0.039 Uiso 1 1 calc R . .
C12 C -0.5421(4) 0.8905(2) 0.6455(3) 0.0339(9) Uani 1 1 d . . .
H12A H -0.6332 0.8858 0.6218 0.041 Uiso 1 1 calc R . .
C13 C -0.5033(4) 0.8657(2) 0.7205(2) 0.0306(9) Uani 1 1 d . . .
H13A H -0.5673 0.8412 0.7481 0.037 Uiso 1 1 calc R . .
C14 C -0.3720(4) 0.87573(19) 0.7566(2) 0.0244(8) Uani 1 1 d . . .
C15 C -0.3271(4) 0.8384(2) 0.8350(2) 0.0271(8) Uani 1 1 d . . .
H15A H -0.3664 0.7913 0.8483 0.032 Uiso 1 1 calc R . .
C16 C -0.2190(4) 0.8768(2) 0.8920(2) 0.0279(8) Uani 1 1 d . . .
H16A H -0.2505 0.9291 0.9032 0.034 Uiso 1 1 calc R . .
H16B H -0.2090 0.8475 0.9416 0.034 Uiso 1 1 calc R . .
C17 C 0.0052(4) 0.9214(2) 0.9318(2) 0.0252(8) Uani 1 1 d . . .
H17A H -0.0002 0.8920 0.9804 0.030 Uiso 1 1 calc R . .
H17B H -0.0298 0.9738 0.9393 0.030 Uiso 1 1 calc R . .
C18 C 0.4924(4) 0.8598(2) 1.0277(2) 0.0319(9) Uani 1 1 d . . .
H18A H 0.5830 0.8728 1.0164 0.048 Uiso 1 1 calc R . .
H18B H 0.4789 0.8040 1.0231 0.048 Uiso 1 1 calc R . .
H18C H 0.4827 0.8762 1.0808 0.048 Uiso 1 1 calc R . .
C19 C -0.0304(4) 0.80641(18) 0.8513(2) 0.0264(8) Uani 1 1 d . . .
H19A H -0.0275 0.7749 0.8986 0.040 Uiso 1 1 calc R . .
H19B H 0.0608 0.8114 0.8373 0.040 Uiso 1 1 calc R . .
H19C H -0.0891 0.7818 0.8083 0.040 Uiso 1 1 calc R . .
C20 C 0.1064(4) 1.0852(3) 0.5311(2) 0.0370(10) Uani 1 1 d . . .
H20A H 0.1343 1.1143 0.4875 0.056 Uiso 1 1 calc R . .
H20B H 0.0083 1.0886 0.5292 0.056 Uiso 1 1 calc R . .
H20C H 0.1326 1.0312 0.5271 0.056 Uiso 1 1 calc R . .
C21 C 0.1415(5) 1.2005(2) 0.6071(3) 0.0379(10) Uani 1 1 d . . .
H21A H 0.1665 1.2249 0.5600 0.057 Uiso 1 1 calc R . .
H21B H 0.1923 1.2243 0.6535 0.057 Uiso 1 1 calc R . .
H21C H 0.0446 1.2073 0.6084 0.057 Uiso 1 1 calc R . .
C22 C 0.0814(4) 0.89454(19) 0.6634(2) 0.0226(7) Uani 1 1 d . . .
C23 C -0.1674(4) 1.0909(2) 0.6320(2) 0.0265(8) Uani 1 1 d . . .
C24 C -0.2149(4) 1.1093(2) 0.8251(2) 0.0236(8) Uani 1 1 d . . .
C25 C 0.1268(4) 1.1689(2) 0.8553(2) 0.0313(8) Uiso 1 1 d . . .
H25A H 0.1020 1.2185 0.8763 0.047 Uiso 1 1 calc R . .
H25B H 0.2252 1.1633 0.8639 0.047 Uiso 1 1 calc R . .
H25C H 0.0856 1.1272 0.8819 0.047 Uiso 1 1 calc R . .
C26 C 0.1224(4) 0.8214(2) 0.6248(3) 0.0361(10) Uani 1 1 d . . .
H26A H 0.0636 0.7791 0.6363 0.054 Uiso 1 1 calc R . .
H26B H 0.2162 0.8089 0.6450 0.054 Uiso 1 1 calc R . .
H26C H 0.1139 0.8291 0.5682 0.054 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
_geom_angle_publ_flag
N1 Ni1 O1 91.97(11) . . ?
N1 Ni1 N6 174.81(12) . . ?
O1 Ni1 N6 88.82(12) . . ?
N1 Ni1 O2 92.31(11) . . ?
O1 Ni1 O2 91.24(10) . . ?
N6 Ni1 O2 92.80(11) . . ?
N1 Ni1 N2 82.64(12) . . ?
O1 Ni1 N2 174.61(11) . . ?
N6 Ni1 N2 96.52(13) . . ?
O2 Ni1 N2 89.16(11) . . ?
N1 Ni1 O4 90.67(11) . . ?
O1 Ni1 O4 84.35(9) . . ?
N6 Ni1 O4 84.31(11) . . ?
O2 Ni1 O4 174.76(11) . . ?
N2 Ni1 O4 95.50(11) . . ?
O3 Ni2 N5 169.97(12) . . ?
O3 Ni2 O1 89.12(10) . . ?
N5 Ni2 O1 92.46(12) . . ?
O3 Ni2 N4 95.21(11) . . ?
N5 Ni2 N4 94.61(12) . . ?
O1 Ni2 N4 92.54(10) . . ?
O3 Ni2 N3 85.25(11) . . ?
N5 Ni2 N3 92.25(12) . . ?
O1 Ni2 N3 172.53(11) . . ?
N4 Ni2 N3 92.86(12) . . ?
O3 Ni2 N6 87.89(11) . . ?
N5 Ni2 N6 82.72(12) . . ?
O1 Ni2 N6 78.65(10) . . ?
N4 Ni2 N6 170.64(11) . . ?
N3 Ni2 N6 96.20(11) . . ?
C1 O1 Ni1 125.1(2) . . ?
C1 O1 Ni2 126.2(2) . . ?
Ni1 O1 Ni2 98.93(9) . . ?
C22 O2 Ni1 124.9(3) . . ?
C22 O3 Ni2 132.4(2) . . ?
C25 O4 Ni1 117.9(2) . . ?
C7 N1 C8 119.2(3) . . ?
C7 N1 Ni1 125.4(3) . . ?
C8 N1 Ni1 114.8(2) . . ?
C21 N2 C9 110.6(3) . . ?
C21 N2 C20 108.0(3) . . ?
C9 N2 C20 108.5(3) . . ?
C21 N2 Ni1 112.2(3) . . ?
C9 N2 Ni1 103.8(2) . . ?
C20 N2 Ni1 113.7(2) . . ?
C14 N3 C10 117.8(3) . . ?
C14 N3 Ni2 126.4(2) . . ?
C10 N3 Ni2 114.9(2) . . ?
C19 N4 C16 110.3(3) . . ?
C19 N4 C17 109.7(3) . . ?
C16 N4 C17 106.0(3) . . ?
C19 N4 Ni2 114.8(2) . . ?
C16 N4 Ni2 108.9(2) . . ?
C17 N4 Ni2 106.7(2) . . ?
C24 N5 Ni2 144.8(3) . . ?
C23 N6 Ni1 140.0(3) . . ?
C23 N6 Ni2 132.4(3) . . ?
Ni1 N6 Ni2 87.48(11) . . ?
O1 C1 C2 119.0(3) . . ?
O1 C1 C6 123.5(3) . . ?
C2 C1 C6 117.5(3) . . ?
C3 C2 C1 120.7(4) . . ?
C3 C2 C17 119.0(3) . . ?
C1 C2 C17 120.2(3) . . ?
C2 C3 C4 122.0(4) . . ?
C5 C4 C3 116.8(3) . . ?
C5 C4 C18 122.4(4) . . ?
C3 C4 C18 120.9(4) . . ?
C4 C5 C6 124.0(4) . . ?
C5 C6 C1 118.9(3) . . ?
C5 C6 C7 115.3(3) . . ?
C1 C6 C7 125.6(3) . . ?
N1 C7 C6 125.6(4) . . ?
N1 C8 C9 106.6(3) . . ?
N2 C9 C8 111.0(4) . . ?
N3 C10 C11 124.0(4) . . ?
C10 C11 C12 117.8(4) . . ?
C13 C12 C11 118.6(4) . . ?
C12 C13 C14 120.9(4) . . ?
N3 C14 C13 120.5(3) . . ?
N3 C14 C15 119.5(3) . . ?
C13 C14 C15 119.7(3) . . ?
C14 C15 C16 119.4(3) . . ?
N4 C16 C15 115.9(3) . . ?
N4 C17 C2 114.5(3) . . ?
O3 C22 O2 127.0(3) . . ?
O3 C22 C26 115.1(3) . . ?
O2 C22 C26 117.9(4) . . ?
N6 C23 S1 177.6(3) . . ?
N5 C24 S2 177.6(4) . . ?
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 N1 1.995(3) . ?
Ni1 O1 2.018(2) . ?
Ni1 N6 2.057(3) . ?
Ni1 O2 2.056(2) . ?
Ni1 N2 2.164(3) . ?
Ni1 O4 2.243(3) . ?
Ni2 O3 1.983(3) . ?
Ni2 N5 2.039(3) . ?
Ni2 O1 2.064(2) . ?
Ni2 N4 2.090(3) . ?
Ni2 N3 2.091(3) . ?
Ni2 N6 2.415(3) . ?
S1 C23 1.616(4) . ?
S2 C24 1.631(4) . ?
O1 C1 1.333(4) . ?
O2 C22 1.266(4) . ?
O3 C22 1.250(5) . ?
O4 C25 1.437(5) . ?
N1 C7 1.286(4) . ?
N1 C8 1.461(5) . ?
N2 C21 1.475(5) . ?
N2 C9 1.486(5) . ?
N2 C20 1.485(5) . ?
N3 C14 1.347(5) . ?
N3 C10 1.350(5) . ?
N4 C19 1.478(4) . ?
N4 C16 1.487(5) . ?
N4 C17 1.498(4) . ?
N5 C24 1.165(4) . ?
N6 C23 1.181(5) . ?
C1 C2 1.411(5) . ?
C1 C6 1.422(5) . ?
C2 C3 1.398(5) . ?
C2 C17 1.505(5) . ?
C3 C4 1.403(6) . ?
C4 C5 1.359(6) . ?
C4 C18 1.523(5) . ?
C5 C6 1.412(5) . ?
C6 C7 1.443(5) . ?
C8 C9 1.524(5) . ?
C10 C11 1.371(5) . ?
C11 C12 1.386(6) . ?
C12 C13 1.370(6) . ?
C13 C14 1.386(5) . ?
C14 C15 1.514(5) . ?
C15 C16 1.515(5) . ?
C22 C26 1.517(5) . ?
