#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:40:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178910 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/39/4113982.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_4113982
loop_
_publ_author_name
'Diran Herebian'
'Eberhard Bothe'
'Frank Neese'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 Molecular and Electronic Structures of
 Bis-(o-diiminobenzosemiquinonato)metal(II) Complexes (Ni, Pd, Pt), Their
 Monocations and -Anions, and of Dimeric Dications Containing Weak
 Metal-Metal Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9116
_journal_page_last               9128
_journal_paper_doi               10.1021/ja030123u
_journal_volume                  125
_journal_year                    2003
_chemical_formula_structural     '[C56 H88 N8 Ni2]2+, 2 (Cl), C4H9NO, 4 H2O'
_chemical_formula_sum            'C60 H105 Cl2 N9 Ni2 O5'
_chemical_formula_weight         1220.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                104.21(2)
_cell_angle_beta                 101.48(2)
_cell_angle_gamma                102.03(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4103(9)
_cell_length_b                   10.4924(9)
_cell_length_c                   16.2202(12)
_cell_measurement_reflns_used    12207
_cell_measurement_temperature    100(2)
_cell_volume                     1620.2(4)
_computing_cell_refinement       'Nonius Collect'
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'Nonius Collect'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '392 images at 1 deg. in ω and 120 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16191
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   'MulScanAbs, Platon99 program suite'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       'small transparent block'
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         9281
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_obs          0.0634
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0587P)²+2.6601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1665
_refine_ls_wR_factor_obs         0.1467
_reflns_number_observed          6861
_reflns_number_total             9341
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030123u_5.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.6601P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+2.6601P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1620.2(2)
_cod_database_code               4113982
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.03439(3) 0.11348(4) 0.46997(2) 0.02418(11) Uani 1 d . .
Cl1 Cl 0.42486(9) 0.17051(11) 0.42972(6) 0.0262(3) Uani 0.707(3) d P 1
O2 O 0.5773(5) 0.1728(5) 0.2696(3) 0.0652(13) Uani 0.707(3) d P 1
Cl1X Cl 0.5790(6) 0.1633(6) 0.3469(4) 0.092(2) Uiso 0.293(3) d P 2
O2X O 0.3848(12) 0.0968(13) 0.4426(7) 0.062(3) Uiso 0.293(3) d P 2
N1 N 0.0899(2) 0.0565(3) 0.36870(14) 0.0240(5) Uani 1 d D .
H1 H 0.1736(22) 0.0695(34) 0.3661(22) 0.029 Uiso 1 d D .
N6 N -0.1360(2) 0.0360(2) 0.39444(14) 0.0232(5) Uani 1 d D .
H6 H -0.2110(24) 0.0314(34) 0.4102(21) 0.028 Uiso 1 d D .
C1 C -0.0074(3) -0.0063(3) 0.2950(2) 0.0204(5) Uani 1 d . .
C2 C 0.0015(3) -0.0584(3) 0.2052(2) 0.0191(5) Uani 1 d . .
C3 C -0.1198(3) -0.1118(3) 0.1415(2) 0.0205(5) Uani 1 d . .
H3 H -0.1157(3) -0.1483(3) 0.0827(2) 0.025 Uiso 1 calc R .
C4 C -0.2536(2) -0.1177(3) 0.1557(2) 0.0187(5) Uani 1 d . .
C5 C -0.2637(3) -0.0725(3) 0.2399(2) 0.0203(5) Uani 1 d . .
H5 H -0.3504(3) -0.0778(3) 0.2513(2) 0.024 Uiso 1 calc R .
C6 C -0.1422(3) -0.0170(3) 0.3107(2) 0.0200(5) Uani 1 d . .
C7 C 0.1387(3) -0.0460(3) 0.1832(2) 0.0212(5) Uani 1 d . .
C8 C 0.2268(3) -0.1183(3) 0.2332(2) 0.0256(6) Uani 1 d . .
H8A H 0.3177(7) -0.0993(18) 0.2232(12) 0.038 Uiso 1 calc R .
H8B H 0.1843(12) -0.2170(4) 0.2119(10) 0.038 Uiso 1 calc R .
H8C H 0.2344(18) -0.0847(16) 0.2964(2) 0.038 Uiso 1 calc R .
C9 C 0.2131(3) 0.1065(3) 0.2043(2) 0.0277(6) Uani 1 d . .
H9A H 0.3001(11) 0.1146(3) 0.1887(14) 0.042 Uiso 1 calc R .
H9B H 0.2300(20) 0.1521(6) 0.2674(3) 0.042 Uiso 1 calc R .
H9C H 0.1566(10) 0.1495(6) 0.1702(11) 0.042 Uiso 1 calc R .
C10 C 0.1205(3) -0.1128(3) 0.0844(2) 0.0276(6) Uani 1 d . .
H10A H 0.2100(3) -0.1052(20) 0.0726(3) 0.041 Uiso 1 calc R .
H10B H 0.0692(20) -0.0663(15) 0.0498(2) 0.041 Uiso 1 calc R .
H10C H 0.0706(20) -0.2094(6) 0.0678(4) 0.041 Uiso 1 calc R .
C11 C -0.3770(3) -0.1722(3) 0.0750(2) 0.0192(5) Uani 1 d . .
C12 C -0.5087(3) -0.1581(3) 0.1000(2) 0.0256(6) Uani 1 d . .
H12A H -0.4986(8) -0.0622(4) 0.1306(12) 0.038 Uiso 1 calc R .
H12B H -0.5276(12) -0.2139(17) 0.1388(11) 0.038 Uiso 1 calc R .
H12C H -0.5842(5) -0.1892(21) 0.0464(2) 0.038 Uiso 1 calc R .
C13 C -0.3926(3) -0.3232(3) 0.0309(2) 0.0294(6) Uani 1 d . .
H13A H -0.4716(14) -0.3584(7) -0.0207(9) 0.044 Uiso 1 calc R .
H13B H -0.4059(23) -0.3747(5) 0.0728(5) 0.044 Uiso 1 calc R .
H13C H -0.3104(10) -0.3333(4) 0.0123(13) 0.044 Uiso 1 calc R .
C14 C -0.3564(3) -0.0933(3) 0.0086(2) 0.0284(6) Uani 1 d . .
H14A H -0.3464(23) 0.0036(5) 0.0362(5) 0.043 Uiso 1 calc R .
H14B H -0.4354(11) -0.1293(16) -0.0430(7) 0.043 Uiso 1 calc R .
H14C H -0.2741(13) -0.1039(19) -0.0099(11) 0.043 Uiso 1 calc R .
N21 N 0.2030(2) 0.2189(3) 0.54521(15) 0.0265(5) Uani 1 d D .
H21 H 0.2782(25) 0.2209(36) 0.5302(22) 0.032 Uiso 1 d D .
N26 N -0.0293(2) 0.1892(3) 0.56213(14) 0.0240(5) Uani 1 d D .
H26 H -0.1144(21) 0.1726(34) 0.5616(22) 0.029 Uiso 1 d D .
C21 C 0.2018(3) 0.2977(3) 0.6221(2) 0.0241(5) Uani 1 d . .
C22 C 0.3119(3) 0.3991(3) 0.6918(2) 0.0242(5) Uani 1 d . .
C23 C 0.2746(3) 0.4746(3) 0.7599(2) 0.0254(6) Uani 1 d . .
H23 H 0.3456(3) 0.5405(3) 0.8064(2) 0.030 Uiso 1 calc R .
C24 C 0.1368(3) 0.4632(3) 0.7677(2) 0.0234(5) Uani 1 d . .
C25 C 0.0328(3) 0.3626(3) 0.7055(2) 0.0228(5) Uani 1 d . .
H25 H -0.0576(3) 0.3480(3) 0.7114(2) 0.027 Uiso 1 calc R .
C26 C 0.0625(3) 0.2798(3) 0.6314(2) 0.0227(5) Uani 1 d . .
C27 C 0.4608(3) 0.4242(3) 0.6866(2) 0.0271(6) Uani 1 d . .
C28 C 0.5580(3) 0.5323(4) 0.7702(2) 0.0374(7) Uani 1 d . .
H28A H 0.5325(17) 0.6184(8) 0.7775(10) 0.056 Uiso 1 calc R .
H28B H 0.6516(4) 0.5467(20) 0.7646(8) 0.056 Uiso 1 calc R .
H28C H 0.5519(20) 0.5006(12) 0.8216(3) 0.056 Uiso 1 calc R .
C29 C 0.5077(3) 0.2926(3) 0.6776(2) 0.0299(6) Uani 1 d . .
H29A H 0.4440(13) 0.2191(7) 0.6275(9) 0.045 Uiso 1 calc R .
H29B H 0.5101(23) 0.2664(13) 0.7317(6) 0.045 Uiso 1 calc R .
H29C H 0.5989(10) 0.3088(8) 0.6679(15) 0.045 Uiso 1 calc R .
C30 C 0.4761(3) 0.4801(4) 0.6084(2) 0.0391(8) Uani 1 d . .
H30A H 0.4448(25) 0.5629(15) 0.6149(9) 0.059 Uiso 1 calc R .
H30B H 0.4213(21) 0.4110(10) 0.5531(3) 0.059 Uiso 1 calc R .
H30C H 0.5720(5) 0.5017(25) 0.6076(10) 0.059 Uiso 1 calc R .
C31 C 0.1119(3) 0.5652(3) 0.8447(2) 0.0285(6) Uani 1 d . .
C32 C 0.1779(4) 0.7119(3) 0.8471(3) 0.0411(8) Uani 1 d . .
H32A H 0.1611(24) 0.7766(3) 0.8960(11) 0.062 Uiso 1 calc R .
H32B H 0.1384(20) 0.7271(9) 0.7914(7) 0.062 Uiso 1 calc R .
H32C H 0.2762(5) 0.7256(9) 0.8555(18) 0.062 Uiso 1 calc R .
C33 C -0.0398(3) 0.5500(3) 0.8369(2) 0.0345(7) Uani 1 d . .
H33A H -0.0507(3) 0.6199(16) 0.8857(9) 0.052 Uiso 1 calc R .
H33B H -0.0828(6) 0.4592(10) 0.8395(16) 0.052 Uiso 1 calc R .
H33C H -0.0830(6) 0.5613(25) 0.7807(7) 0.052 Uiso 1 calc R .
C34 C 0.1752(3) 0.5415(3) 0.9320(2) 0.0335(7) Uani 1 d . .
H34A H 0.1622(21) 0.6087(15) 0.9813(2) 0.050 Uiso 1 calc R .
H34B H 0.2727(6) 0.5517(24) 0.9386(8) 0.050 Uiso 1 calc R .
H34C H 0.1308(17) 0.4492(9) 0.9316(7) 0.050 Uiso 1 calc R .
O1 O -0.3210(3) 0.0853(3) 0.5083(2) 0.0561(7) Uani 1 d D .
H1A H -0.3023(49) 0.1880(39) 0.5514(29) 0.073 Uiso 1 d D .
H1B H -0.4024(42) 0.0945(50) 0.4583(27) 0.073 Uiso 1 d D .
O50 O 0.1733(10) 0.5528(12) 0.4879(7) 0.114(3) Uani 0.50 d P .
C51 C 0.1029(8) 0.5800(9) 0.5523(6) 0.039(2) Uiso 0.50 d P .
C52 C 0.1453(6) 0.6827(6) 0.6314(4) 0.0288(12) Uani 0.50 d P .
H52A H 0.2444(6) 0.7196(6) 0.6467(4) 0.043 Uiso 0.50 calc PR .
H52B H 0.1200(6) 0.6459(6) 0.6777(4) 0.043 Uiso 0.50 calc PR .
H52C H 0.1017(6) 0.7556(6) 0.6262(4) 0.043 Uiso 0.50 calc PR .
N53 N -0.0353(8) 0.5187(9) 0.5227(5) 0.092(4) Uani 0.50 d PD .
C54 C -0.0807(16) 0.3982(15) 0.4283(9) 0.089(5) Uiso 0.50 d PD .
H54A H -0.1796(16) 0.3592(15) 0.4113(9) 0.134 Uiso 0.50 calc PR .
H54B H -0.0356(16) 0.3264(15) 0.4341(9) 0.134 Uiso 0.50 calc PR .
H54C H -0.0540(16) 0.4367(15) 0.3830(9) 0.134 Uiso 0.50 calc PR .
C55 C -0.1209(9) 0.5723(11) 0.5920(6) 0.061(2) Uani 0.50 d PD .
H55A H -0.2179(9) 0.5247(11) 0.5668(6) 0.091 Uiso 0.50 calc PR .
H55B H -0.1081(9) 0.6708(11) 0.6031(6) 0.091 Uiso 0.50 calc PR .
H55C H -0.0881(9) 0.5535(11) 0.6475(6) 0.091 Uiso 0.50 calc PR .
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'
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'
O O 0.0106 0.0060 '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_3
N26 Ni1 N6 93.71(10) .
N26 Ni1 N1 171.00(11) .
N6 Ni1 N1 83.17(10) .
N26 Ni1 N21 83.32(10) .
N6 Ni1 N21 170.79(11) .
N1 Ni1 N21 98.44(10) .
N26 Ni1 Ni1 80.39(8) 2_556
N6 Ni1 Ni1 82.62(8) 2_556
N1 Ni1 Ni1 107.47(8) 2_556
N21 Ni1 Ni1 105.37(8) 2_556
C1 N1 Ni1 116.5(2) .
C6 N6 Ni1 116.6(2) .
N1 C1 C2 130.1(2) .
N1 C1 C6 111.3(2) .
C2 C1 C6 118.5(2) .
C3 C2 C1 116.0(2) .
C3 C2 C7 122.4(2) .
C1 C2 C7 121.5(2) .
C2 C3 C4 126.0(2) .
C5 C4 C3 118.5(2) .
C5 C4 C11 123.2(2) .
C3 C4 C11 118.3(2) .
C4 C5 C6 119.2(2) .
N6 C6 C5 125.8(2) .
N6 C6 C1 112.5(2) .
C5 C6 C1 121.6(2) .
C2 C7 C10 111.3(2) .
C2 C7 C8 111.6(2) .
C10 C7 C8 106.5(2) .
C2 C7 C9 109.4(2) .
C10 C7 C9 107.0(2) .
C8 C7 C9 111.0(2) .
C13 C11 C12 108.6(2) .
C13 C11 C4 109.3(2) .
C12 C11 C4 111.9(2) .
C13 C11 C14 108.8(2) .
C12 C11 C14 108.2(2) .
C4 C11 C14 110.0(2) .
C21 N21 Ni1 116.4(2) .
C26 N26 Ni1 116.3(2) .
N21 C21 C22 130.4(3) .
N21 C21 C26 110.8(2) .
C22 C21 C26 118.7(2) .
C23 C22 C21 116.0(2) .
C23 C22 C27 122.2(2) .
C21 C22 C27 121.7(2) .
C22 C23 C24 125.9(3) .
C25 C24 C23 118.7(2) .
C25 C24 C31 122.2(2) .
C23 C24 C31 119.1(2) .
C24 C25 C26 118.9(2) .
N26 C26 C25 125.2(2) .
N26 C26 C21 113.0(2) .
C25 C26 C21 121.6(2) .
C28 C27 C22 111.4(2) .
C28 C27 C29 107.0(2) .
C22 C27 C29 111.2(2) .
C28 C27 C30 106.7(3) .
C22 C27 C30 109.7(2) .
C29 C27 C30 110.7(3) .
C33 C31 C32 108.0(3) .
C33 C31 C24 112.3(2) .
C32 C31 C24 109.8(3) .
C33 C31 C34 108.0(3) .
C32 C31 C34 109.3(3) .
C24 C31 C34 109.4(2) .
C52 C51 N53 115.6(8) .
C52 C51 O50 128.2(8) .
N53 C51 O50 114.0(8) .
C51 N53 C55 113.9(8) .
C51 N53 C54 113.8(8) .
C55 N53 C54 132.2(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N26 1.827(2) .
Ni1 N6 1.831(2) .
Ni1 N1 1.852(2) .
Ni1 N21 1.863(2) .
Ni1 Ni1 2.7996(9) 2_556
N1 C1 1.320(3) .
N6 C6 1.318(3) .
C1 C2 1.455(3) .
C1 C6 1.462(3) .
C2 C3 1.370(4) .
C2 C7 1.527(3) .
C3 C4 1.448(3) .
C4 C5 1.364(3) .
C4 C11 1.531(3) .
C5 C6 1.431(3) .
C7 C10 1.538(4) .
C7 C8 1.540(4) .
C7 C9 1.545(4) .
C11 C13 1.529(4) .
C11 C12 1.530(4) .
C11 C14 1.533(4) .
N21 C21 1.321(3) .
N26 C26 1.323(3) .
C21 C22 1.452(4) .
C21 C26 1.465(4) .
C22 C23 1.367(4) .
C22 C27 1.540(4) .
C23 C24 1.448(4) .
C24 C25 1.368(4) .
C24 C31 1.536(4) .
C25 C26 1.428(4) .
C27 C28 1.539(4) .
C27 C29 1.542(4) .
C27 C30 1.543(4) .
C31 C33 1.530(4) .
C31 C32 1.536(5) .
C31 C34 1.540(4) .
O50 C51 1.398(13) .
C51 C52 1.379(11) .
C51 N53 1.380(11) .
N53 C55 1.634(9) .
N53 C54 1.637(10) .
