#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/49/7104930.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_7104930
loop_
_publ_author_name
'Mondal, Amrita'
'Weyhermüller, Thomas'
'Wieghardt, Karl'
_publ_section_title
;
 Redox-noninnocence of
 N,N'-bis(6-methyl-2-pyridylmethylene)ethane-1,2-diamine (L): synthesis
 and characterization of diamagnetic [Ni(II)2(L**)2] and
 [Zn(II)2(L)Cl4]((L**)2- pi diradical dianion of L).
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6098
_journal_page_last               6100
_journal_paper_doi               10.1039/b912604j
_journal_year                    2009
_chemical_formula_moiety         'C32 H36 N8 Ni2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C34 H41 N8 Ni2 O0.5'
_chemical_formula_weight         687.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.060(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.529(2)
_cell_length_b                   8.8499(9)
_cell_length_c                   20.938(2)
_cell_measurement_reflns_used    9539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.740
_cell_measurement_theta_min      2.813
_cell_volume                     3223.5(6)
_computing_cell_refinement       'Bruker SAINT 7.34a'
_computing_data_collection       'Bruker SAINT 7.34a'
_computing_data_reduction        'Bruker SAINT 7.34a'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode + INCOATEC Muti-Layer-Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            96839
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  0.9647
_exptl_absorpt_correction_T_min  0.8492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Vers. 2008/1, Bruker AXS (2008)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         11664
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0288
_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)+(0.0338P)²+1.3089P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                10026
_reflns_number_total             11664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b912604j.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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)/c
_cod_original_formula_sum        'C34 H41 N8 Ni2 O0.50'
_cod_database_code               7104930
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.168605(8) 0.347474(15) 0.181745(7) 0.01698(4) Uani 1 1 d . . .
Ni2 Ni 0.323278(8) 0.553304(16) 0.096727(7) 0.01719(4) Uani 1 1 d . . .
N1 N 0.05693(6) 0.33504(10) 0.17294(5) 0.01831(17) Uani 1 1 d . . .
C2 C 0.01143(7) 0.21028(13) 0.16902(6) 0.0221(2) Uani 1 1 d . . .
C3 C -0.06739(7) 0.22016(16) 0.16746(6) 0.0288(3) Uani 1 1 d . . .
H3 H -0.0975 0.1307 0.1659 0.035 Uiso 1 1 calc R . .
C4 C -0.10309(7) 0.36192(17) 0.16817(6) 0.0294(3) Uani 1 1 d . . .
H4 H -0.1573 0.3696 0.1673 0.035 Uiso 1 1 calc R . .
C5 C -0.05843(7) 0.48880(16) 0.17015(6) 0.0268(2) Uani 1 1 d . . .
H5 H -0.0814 0.5861 0.1695 0.032 Uiso 1 1 calc R . .
C6 C 0.02193(7) 0.47430(13) 0.17320(6) 0.0206(2) Uani 1 1 d . . .
C7 C 0.07464(7) 0.59576(13) 0.17896(6) 0.0220(2) Uani 1 1 d . . .
H7 H 0.0580 0.6979 0.1792 0.026 Uiso 1 1 calc R . .
N8 N 0.14838(6) 0.55973(10) 0.18396(5) 0.01982(17) Uani 1 1 d . . .
C9 C 0.20301(7) 0.68552(13) 0.19034(6) 0.0246(2) Uani 1 1 d . . .
H9A H 0.1808 0.7702 0.2128 0.029 Uiso 1 1 calc R . .
H9B H 0.2114 0.7212 0.1469 0.029 Uiso 1 1 calc R . .
C10 C 0.27968(7) 0.64146(14) 0.22725(6) 0.0247(2) Uani 1 1 d . . .
H10A H 0.3083 0.7341 0.2419 0.030 Uiso 1 1 calc R . .
H10B H 0.2705 0.5829 0.2659 0.030 Uiso 1 1 calc R . .
N11 N 0.32637(6) 0.55116(11) 0.18822(5) 0.02049(17) Uani 1 1 d . . .
C12 C 0.37930(7) 0.46136(13) 0.21847(6) 0.0222(2) Uani 1 1 d . . .
H12 H 0.3844 0.4478 0.2638 0.027 Uiso 1 1 calc R . .
C13 C 0.42783(6) 0.38654(13) 0.17934(5) 0.01980(19) Uani 1 1 d . . .
C14 C 0.48981(7) 0.29135(14) 0.20170(6) 0.0244(2) Uani 1 1 d . . .
H14 H 0.5007 0.2684 0.2462 0.029 Uiso 1 1 calc R . .
C15 C 0.53422(7) 0.23234(14) 0.15834(7) 0.0264(2) Uani 1 1 d . . .
H15 H 0.5772 0.1705 0.1727 0.032 Uiso 1 1 calc R . .
C16 C 0.51567(6) 0.26403(13) 0.09253(6) 0.0233(2) Uani 1 1 d . . .
H16 H 0.5463 0.2243 0.0621 0.028 Uiso 1 1 calc R . .
C17 C 0.45267(6) 0.35320(12) 0.07228(6) 0.01826(19) Uani 1 1 d . . .
N18 N 0.40952(5) 0.41715(10) 0.11483(5) 0.01747(16) Uani 1 1 d . . .
C19 C 0.05172(8) 0.06160(14) 0.16609(7) 0.0289(2) Uani 1 1 d . . .
H19A H 0.0744 0.0547 0.1257 0.043 Uiso 1 1 calc R . .
H19B H 0.0147 -0.0207 0.1682 0.043 Uiso 1 1 calc R . .
H19C H 0.0924 0.0536 0.2025 0.043 Uiso 1 1 calc R . .
C20 C 0.42655(7) 0.38106(14) 0.00246(6) 0.0219(2) Uani 1 1 d . . .
H20A H 0.3777 0.3287 -0.0100 0.033 Uiso 1 1 calc R . .
H20B H 0.4653 0.3429 -0.0234 0.033 Uiso 1 1 calc R . .
H20C H 0.4195 0.4898 -0.0049 0.033 Uiso 1 1 calc R . .
N21 N 0.23176(5) 0.23632(10) 0.24879(5) 0.01786(16) Uani 1 1 d . . .
C22 C 0.22957(6) 0.23797(12) 0.31361(6) 0.01944(19) Uani 1 1 d . . .
C23 C 0.27810(7) 0.15098(14) 0.35540(6) 0.0249(2) Uani 1 1 d . . .
H23 H 0.2741 0.1528 0.4002 0.030 Uiso 1 1 calc R . .
C24 C 0.33379(8) 0.05920(14) 0.33125(7) 0.0280(2) Uani 1 1 d . . .
H24 H 0.3679 -0.0007 0.3595 0.034 Uiso 1 1 calc R . .
C25 C 0.33786(7) 0.05779(13) 0.26628(7) 0.0251(2) Uani 1 1 d . . .
H25 H 0.3756 -0.0018 0.2492 0.030 Uiso 1 1 calc R . .
C26 C 0.28585(6) 0.14513(12) 0.22513(6) 0.01970(19) Uani 1 1 d . . .
C27 C 0.28249(7) 0.15077(12) 0.15708(6) 0.0213(2) Uani 1 1 d . . .
H27 H 0.3163 0.0932 0.1345 0.026 Uiso 1 1 calc R . .
N28 N 0.22975(6) 0.24062(10) 0.12702(5) 0.01947(17) Uani 1 1 d . . .
C29 C 0.22102(8) 0.23990(13) 0.05656(6) 0.0243(2) Uani 1 1 d . . .
H29A H 0.1885 0.1530 0.0406 0.029 Uiso 1 1 calc R . .
H29B H 0.2721 0.2266 0.0418 0.029 Uiso 1 1 calc R . .
C30 C 0.18491(7) 0.38456(13) 0.02824(6) 0.0222(2) Uani 1 1 d . . .
H30A H 0.1651 0.3670 -0.0175 0.027 Uiso 1 1 calc R . .
H30B H 0.1407 0.4113 0.0513 0.027 Uiso 1 1 calc R . .
N31 N 0.23876(5) 0.51139(11) 0.03239(5) 0.01896(17) Uani 1 1 d . . .
C32 C 0.22877(6) 0.61161(13) -0.01480(6) 0.0208(2) Uani 1 1 d . . .
H32 H 0.1897 0.6002 -0.0502 0.025 Uiso 1 1 calc R . .
C33 C 0.27947(6) 0.73679(12) -0.00972(6) 0.01967(19) Uani 1 1 d . . .
C34 C 0.27772(7) 0.85546(13) -0.05452(6) 0.0243(2) Uani 1 1 d . . .
H34 H 0.2409 0.8552 -0.0918 0.029 Uiso 1 1 calc R . .
C35 C 0.32955(8) 0.97167(13) -0.04389(7) 0.0259(2) Uani 1 1 d . . .
H35 H 0.3293 1.0528 -0.0736 0.031 Uiso 1 1 calc R . .
C36 C 0.38330(7) 0.96806(13) 0.01211(6) 0.0237(2) Uani 1 1 d . . .
H36 H 0.4195 1.0476 0.0204 0.028 Uiso 1 1 calc R . .
C37 C 0.38335(6) 0.84945(12) 0.05469(6) 0.01960(19) Uani 1 1 d . . .
N38 N 0.33230(5) 0.73313(10) 0.04472(5) 0.01768(16) Uani 1 1 d . . .
C39 C 0.17244(7) 0.34401(13) 0.33703(6) 0.0236(2) Uani 1 1 d . . .
H39A H 0.1889 0.4485 0.3314 0.035 Uiso 1 1 calc R . .
H39B H 0.1692 0.3250 0.3827 0.035 Uiso 1 1 calc R . .
H39C H 0.1219 0.3279 0.3123 0.035 Uiso 1 1 calc R . .
C40 C 0.43891(7) 0.84020(14) 0.11509(6) 0.0254(2) Uani 1 1 d . . .
H40A H 0.4104 0.8383 0.1525 0.038 Uiso 1 1 calc R . .
H40B H 0.4729 0.9284 0.1178 0.038 Uiso 1 1 calc R . .
H40C H 0.4696 0.7479 0.1144 0.038 Uiso 1 1 calc R . .
C41 C 0.0263(2) 0.7177(4) 0.00863(19) 0.0383(7) Uani 0.50 1 d PD . .
H41A H 0.0697 0.6472 0.0114 0.057 Uiso 0.50 1 calc PR . .
H41B H -0.0100 0.6939 -0.0295 0.057 Uiso 0.50 1 calc PR . .
H41C H 0.0003 0.7083 0.0473 0.057 Uiso 0.50 1 calc PR . .
C42 C 0.05524(14) 0.8766(3) 0.00348(14) 0.0303(5) Uani 0.50 1 d PD . .
H42A H 0.0922 0.9012 0.0417 0.036 Uiso 0.50 1 calc PR . .
H42B H 0.0821 0.8866 -0.0352 0.036 Uiso 0.50 1 calc PR . .
O43 O -0.0077(2) 0.9769(2) -0.0007(3) 0.0305(7) Uani 0.50 1 d PD . .
C45 C -0.0576(3) 1.2253(5) -0.0154(2) 0.0535(10) Uani 0.50 1 d PD . .
H45A H -0.0437 1.3307 -0.0225 0.080 Uiso 0.50 1 calc PR . .
H45B H -0.0808 1.2176 0.0247 0.080 Uiso 0.50 1 calc PR . .
H45C H -0.0946 1.1909 -0.0514 0.080 Uiso 0.50 1 calc PR . .
C44 C 0.01321(18) 1.1284(4) -0.01098(16) 0.0381(6) Uani 0.50 1 d PD . .
H44A H 0.0371 1.1362 -0.0513 0.046 Uiso 0.50 1 calc PR . .
H44B H 0.0510 1.1632 0.0250 0.046 Uiso 0.50 1 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'
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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N28 Ni1 N8 128.25(4) . . ?
N28 Ni1 N21 82.59(4) . . ?
N8 Ni1 N21 124.74(4) . . ?
N28 Ni1 N1 123.12(4) . . ?
N8 Ni1 N1 82.57(4) . . ?
N21 Ni1 N1 121.09(4) . . ?
N11 Ni2 N31 128.96(4) . . ?
N11 Ni2 N18 82.65(4) . . ?
N31 Ni2 N18 122.45(4) . . ?
N11 Ni2 N38 125.12(4) . . ?
N31 Ni2 N38 82.74(4) . . ?
N18 Ni2 N38 120.26(4) . . ?
C2 N1 C6 117.98(10) . . ?
C2 N1 Ni1 128.88(8) . . ?
C6 N1 Ni1 113.10(7) . . ?
N1 C2 C3 121.88(12) . . ?
N1 C2 C19 116.11(11) . . ?
C3 C2 C19 122.00(11) . . ?
C2 C3 C4 120.18(12) . . ?
C5 C4 C3 118.72(12) . . ?
C4 C5 C6 119.51(12) . . ?
N1 C6 C5 121.67(11) . . ?
N1 C6 C7 113.23(10) . . ?
C5 C6 C7 125.07(11) . . ?
N8 C7 C6 116.47(10) . . ?
C7 N8 C9 116.47(10) . . ?
C7 N8 Ni1 114.63(8) . . ?
C9 N8 Ni1 128.90(8) . . ?
N8 C9 C10 112.32(10) . . ?
N11 C10 C9 112.16(10) . . ?
C12 N11 C10 117.92(10) . . ?
C12 N11 Ni2 114.72(8) . . ?
C10 N11 Ni2 127.30(8) . . ?
N11 C12 C13 116.09(10) . . ?
N18 C13 C14 121.42(11) . . ?
N18 C13 C12 113.06(10) . . ?
C14 C13 C12 125.52(11) . . ?
C15 C14 C13 119.05(11) . . ?
C14 C15 C16 119.48(11) . . ?
C17 C16 C15 119.69(12) . . ?
N18 C17 C16 121.63(11) . . ?
N18 C17 C20 116.28(9) . . ?
C16 C17 C20 122.06(11) . . ?
C17 N18 C13 118.64(10) . . ?
C17 N18 Ni2 127.94(8) . . ?
C13 N18 Ni2 113.41(8) . . ?
C22 N21 C26 117.88(10) . . ?
C22 N21 Ni1 129.08(7) . . ?
C26 N21 Ni1 113.04(8) . . ?
N21 C22 C23 122.39(11) . . ?
N21 C22 C39 115.75(10) . . ?
C23 C22 C39 121.84(11) . . ?
C22 C23 C24 119.63(12) . . ?
C25 C24 C23 118.93(11) . . ?
C24 C25 C26 119.61(11) . . ?
N21 C26 C25 121.53(11) . . ?
N21 C26 C27 113.16(10) . . ?
C25 C26 C27 125.31(11) . . ?
N28 C27 C26 116.12(10) . . ?
C27 N28 C29 117.29(10) . . ?
C27 N28 Ni1 115.07(8) . . ?
C29 N28 Ni1 127.50(8) . . ?
N28 C29 C30 112.16(9) . . ?
N31 C30 C29 112.93(10) . . ?
C32 N31 C30 116.42(10) . . ?
C32 N31 Ni2 114.58(8) . . ?
C30 N31 Ni2 129.00(8) . . ?
N31 C32 C33 116.37(10) . . ?
N38 C33 C34 121.79(10) . . ?
N38 C33 C32 113.30(10) . . ?
C34 C33 C32 124.91(11) . . ?
C35 C34 C33 119.47(11) . . ?
C34 C35 C36 118.61(11) . . ?
C37 C36 C35 120.16(11) . . ?
N38 C37 C36 121.89(11) . . ?
N38 C37 C40 115.70(10) . . ?
C36 C37 C40 122.41(10) . . ?
C37 N38 C33 118.08(10) . . ?
C37 N38 Ni2 128.97(8) . . ?
C33 N38 Ni2 112.93(7) . . ?
O43 C42 C41 109.0(2) . . ?
C42 O43 C44 113.1(3) . . ?
O43 C44 C45 108.9(3) . . ?
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 N28 1.9125(10) . ?
Ni1 N8 1.9132(9) . ?
Ni1 N21 1.9447(10) . ?
Ni1 N1 1.9467(10) . ?
Ni2 N11 1.9098(10) . ?
Ni2 N31 1.9123(10) . ?
Ni2 N18 1.9340(10) . ?
Ni2 N38 1.9457(10) . ?
N1 C2 1.3585(15) . ?
N1 C6 1.3769(14) . ?
C2 C3 1.3808(18) . ?
C2 C19 1.4982(18) . ?
C3 C4 1.403(2) . ?
C4 C5 1.367(2) . ?
C5 C6 1.4081(16) . ?
C6 C7 1.4128(17) . ?
C7 N8 1.3231(15) . ?
N8 C9 1.4637(15) . ?
C9 C10 1.5167(19) . ?
C10 N11 1.4632(15) . ?
N11 C12 1.3225(16) . ?
C12 C13 1.4160(17) . ?
C13 N18 1.3763(14) . ?
C13 C14 1.4085(16) . ?
C14 C15 1.370(2) . ?
C15 C16 1.4046(19) . ?
C16 C17 1.3809(15) . ?
C17 N18 1.3608(15) . ?
C17 C20 1.4976(16) . ?
N21 C22 1.3627(15) . ?
N21 C26 1.3824(14) . ?
C22 C23 1.3781(16) . ?
C22 C39 1.4981(16) . ?
C23 C24 1.4107(18) . ?
C24 C25 1.371(2) . ?
C25 C26 1.4063(17) . ?
C26 C27 1.4197(17) . ?
C27 N28 1.3191(15) . ?
N28 C29 1.4645(15) . ?
C29 C30 1.5162(17) . ?
C30 N31 1.4622(15) . ?
N31 C32 1.3232(15) . ?
C32 C33 1.4160(16) . ?
C33 N38 1.3778(14) . ?
C33 C34 1.4059(16) . ?
C34 C35 1.3722(18) . ?
C35 C36 1.4113(18) . ?
C36 C37 1.3771(16) . ?
C37 N38 1.3632(14) . ?
C37 C40 1.5007(17) . ?
C41 C42 1.504(4) . ?
C42 O43 1.410(4) . ?
O43 C44 1.413(3) . ?
C45 C44 1.503(4) . ?
