#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:00:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180407 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/76/7207645.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_7207645
loop_
_publ_author_name
'Lin, Jiao-Min'
'Qiu, Yan-Xuan'
'Chen, Wen-Bin'
'Yang, Meng'
'Zhou, Ai-Ju'
'Dong, Wen'
'Tian, Chang-En'
_publ_section_title
;
 Unusual π−--π− stacking interactions between
 5,5′-azotetrazolate(AT) anions in six AT based 3d metal
 photochromic complexes
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              2779
_journal_paper_doi               10.1039/c2ce06606h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C10 H28 N26 Ni O2'
_chemical_formula_weight         603.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 98.464(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9182(3)
_cell_length_b                   7.2555(2)
_cell_length_c                   14.5570(4)
_cell_measurement_reflns_used    2882
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.490
_cell_measurement_theta_min      2.81
_cell_volume                     1245.07(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      296(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7608
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0014(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+0.6029P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                2398
_reflns_number_total             2696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06606h.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7207645
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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 0.71371(4) 0.7500 0.01970(11) Uani 1 2 d S
N5 N 0.96522(12) 0.7391(2) 0.77846(11) 0.0255(3) Uani 1 1 d .
N9 N 0.80590(13) 0.2238(2) 0.79922(12) 0.0307(4) Uani 1 1 d .
N3 N 0.67465(12) 0.7180(2) 0.72504(11) 0.0245(3) Uani 1 1 d .
O1 O 0.85247(12) 0.9015(2) 0.97571(12) 0.0359(3) Uani 1 1 d D
C2 C 0.85176(15) 0.2040(2) 0.72193(13) 0.0258(4) Uani 1 1 d .
N10 N 0.96727(13) 0.2016(2) 0.71202(11) 0.0284(3) Uani 1 1 d .
N7 N 0.67456(14) 0.1960(3) 0.67953(13) 0.0367(4) Uani 1 1 d .
N6 N 0.77351(14) 0.1869(3) 0.64694(12) 0.0356(4) Uani 1 1 d .
N8 N 0.69409(14) 0.2193(2) 0.77095(13) 0.0339(4) Uani 1 1 d .
N11 N 0.54042(13) 0.9022(2) 0.85906(11) 0.0262(3) Uani 1 1 d D
N12 N 0.53998(12) 0.5187(2) 0.85561(11) 0.0261(3) Uani 1 1 d D
C3 C 0.55356(16) 0.8016(3) 0.94823(14) 0.0305(4) Uani 1 1 d D
C4 C 0.60430(15) 0.6121(3) 0.93658(13) 0.0292(4) Uani 1 1 d D
N2 N 0.70186(12) 0.6880(3) 0.64163(12) 0.0343(4) Uani 1 1 d .
N1 N 0.81422(12) 0.6952(2) 0.64606(12) 0.0327(4) Uani 1 1 d .
N4 N 0.76837(12) 0.7449(2) 0.78605(11) 0.0257(3) Uani 1 1 d .
C1 C 0.85161(14) 0.7301(2) 0.73513(13) 0.0229(4) Uani 1 1 d .
N13 N 0.93036(14) 0.2686(2) 0.98473(12) 0.0282(4) Uani 1 1 d D
H6 H 0.6816(13) 0.622(3) 0.9251(14) 0.029(5) Uiso 1 1 d D
H5 H 0.6078(18) 0.542(3) 0.9924(12) 0.037(6) Uiso 1 1 d D
H3 H 0.4803(14) 0.788(3) 0.9664(14) 0.025(5) Uiso 1 1 d D
H4 H 0.6004(17) 0.873(3) 0.9956(13) 0.035(6) Uiso 1 1 d D
H2 H 0.4858(15) 0.988(3) 0.8558(15) 0.032(6) Uiso 1 1 d D
H1 H 0.6039(15) 0.959(3) 0.8541(16) 0.040(6) Uiso 1 1 d D
C5 C 0.95984(17) 0.4587(3) 0.96158(15) 0.0336(4) Uiso 1 1 d D
H8 H 0.5776(17) 0.426(3) 0.8366(15) 0.037(6) Uiso 1 1 d D
H7 H 0.4760(14) 0.474(3) 0.8674(14) 0.030(5) Uiso 1 1 d D
H9 H 0.820(2) 0.875(4) 1.0182(12) 0.057(9) Uiso 1 1 d D
H12 H 0.9933(19) 0.451(3) 0.9062(13) 0.053(7) Uiso 1 1 d D
H11 H 0.8951(16) 0.532(3) 0.9504(17) 0.049(7) Uiso 1 1 d D
H13 H 0.890(2) 0.221(3) 0.9384(15) 0.049(7) Uiso 1 1 d D
H14 H 0.9906(18) 0.199(3) 0.9996(19) 0.051(7) Uiso 1 1 d D
H10 H 0.818(2) 0.870(4) 0.9260(11) 0.066(9) Uiso 1 1 d D
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'
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
N12 Ni1 N12 94.89(9) 2_656 .
N12 Ni1 N11 178.13(6) 2_656 .
N12 Ni1 N11 83.26(6) . .
N12 Ni1 N11 83.26(6) 2_656 2_656
N12 Ni1 N11 178.13(6) . 2_656
N11 Ni1 N11 98.59(9) . 2_656
N12 Ni1 N3 90.40(6) 2_656 .
N12 Ni1 N3 90.72(6) . .
N11 Ni1 N3 89.90(6) . .
N11 Ni1 N3 89.02(6) 2_656 .
N12 Ni1 N3 90.72(6) 2_656 2_656
N12 Ni1 N3 90.40(6) . 2_656
N11 Ni1 N3 89.02(6) . 2_656
N11 Ni1 N3 89.90(6) 2_656 2_656
N3 Ni1 N3 178.35(8) . 2_656
N5 N5 C1 112.90(19) 2_756 .
C2 N9 N8 104.63(16) . .
N2 N3 N4 109.95(14) . .
N2 N3 Ni1 121.62(11) . .
N4 N3 Ni1 128.41(12) . .
H9 O1 H10 112(2) . .
N9 C2 N6 112.21(17) . .
N9 C2 N10 128.27(17) . .
N6 C2 N10 119.52(17) . .
N10 N10 C2 113.6(2) 2_756 .
N8 N7 N6 109.19(15) . .
C2 N6 N7 104.61(16) . .
N7 N8 N9 109.37(17) . .
C3 N11 Ni1 109.02(12) . .
C3 N11 H2 111.8(14) . .
Ni1 N11 H2 109.3(14) . .
C3 N11 H1 109.0(15) . .
Ni1 N11 H1 110.5(15) . .
H2 N11 H1 107(2) . .
C4 N12 Ni1 108.18(12) . .
C4 N12 H8 112.1(15) . .
Ni1 N12 H8 111.1(15) . .
C4 N12 H7 112.6(14) . .
Ni1 N12 H7 106.7(14) . .
H8 N12 H7 106(2) . .
N11 C3 C4 109.93(16) . .
N11 C3 H3 108.2(13) . .
C4 C3 H3 109.5(12) . .
N11 C3 H4 109.8(13) . .
C4 C3 H4 111.3(13) . .
H3 C3 H4 108.1(18) . .
N12 C4 C3 109.66(14) . .
N12 C4 H6 107.0(12) . .
C3 C4 H6 111.2(13) . .
N12 C4 H5 112.8(14) . .
C3 C4 H5 110.9(13) . .
H6 C4 H5 105.2(18) . .
N3 N2 N1 109.28(15) . .
C1 N1 N2 104.15(15) . .
C1 N4 N3 103.75(15) . .
N4 C1 N1 112.86(15) . .
N4 C1 N5 119.63(16) . .
N1 C1 N5 127.34(17) . .
C5 N13 H13 109.2(18) . .
C5 N13 H14 112.4(17) . .
H13 N13 H14 108(2) . .
N13 C5 C5 110.7(2) . 3_767
N13 C5 H12 106.4(16) . .
C5 C5 H12 110.9(15) 3_767 .
N13 C5 H11 110.7(16) . .
C5 C5 H11 109.1(15) 3_767 .
H12 C5 H11 109(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N12 2.0921(16) 2_656
Ni1 N12 2.0921(16) .
Ni1 N11 2.0970(16) .
Ni1 N11 2.0970(16) 2_656
Ni1 N3 2.1653(14) .
Ni1 N3 2.1653(14) 2_656
N5 N5 1.256(3) 2_756
N5 C1 1.409(2) .
N9 C2 1.329(3) .
N9 N8 1.336(2) .
N3 N2 1.320(2) .
N3 N4 1.335(2) .
O1 H9 0.802(16) .
O1 H10 0.809(16) .
C2 N6 1.333(2) .
C2 N10 1.405(2) .
N10 N10 1.256(3) 2_756
N7 N8 1.328(3) .
N7 N6 1.336(2) .
N11 C3 1.477(3) .
N11 H2 0.898(15) .
N11 H1 0.874(16) .
N12 C4 1.473(2) .
N12 H8 0.876(16) .
N12 H7 0.869(15) .
C3 C4 1.521(3) .
C3 H3 0.954(15) .
C3 H4 0.970(16) .
C4 H6 0.963(15) .
C4 H5 0.954(15) .
N2 N1 1.332(2) .
N1 C1 1.332(2) .
N4 C1 1.327(2) .
N13 C5 1.475(3) .
N13 H13 0.846(17) .
N13 H14 0.879(17) .
C5 C5 1.487(4) 3_767
C5 H12 0.952(16) .
C5 H11 0.931(16) .
