#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:47:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179674 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/26/4512613.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_4512613
loop_
_publ_author_name
'Zheng, Sheng-Run'
'Pan, Mei'
'Wu, Kai'
'Chen, Ling'
'Jiang, Ji-Jun'
'Wang, Da-Wei'
'Shi, Jian-Ying'
'Su, Cheng-Yong'
_publ_section_title
;
 Assembly of Binuclear, Tetranuclear, and Multinuclear Complexes from
 Pincer-Like Mononuclear Metallotectons: Structural Diversity Dependent on
 Precursors
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              625
_journal_paper_doi               10.1021/cg501306n
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C21 H22 N8 Ni O6'
_chemical_formula_weight         541.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 114.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.888(3)
_cell_length_b                   11.648(2)
_cell_length_c                   14.253(3)
_cell_measurement_reflns_used    4740
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.951
_cell_measurement_theta_min      2.310
_cell_volume                     2243.2(9)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.088
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0168
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7755
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_T_max  0.7821
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0359
_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)+(0.0641P)²+1.4539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2137
_reflns_number_total             2437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501306n_si_001.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4512610--4512617.cif.
;
_cod_original_cell_volume        2243.1(8)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4512613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ni1 Ni 0.5000 -0.30821(3) 0.7500 0.03497(16) Uani 1 2 d S
N2 N 0.62214(14) -0.20364(15) 0.82493(15) 0.0361(4) Uani 1 1 d .
N1 N 0.78617(14) -0.19769(16) 0.88630(15) 0.0394(4) Uani 1 1 d .
H1A H 0.8460 -0.2207 0.9040 0.047 Uiso 1 1 calc R
N3 N 0.61259(15) -0.42848(16) 0.79418(15) 0.0407(4) Uani 1 1 d .
C8 C 0.69994(17) -0.38796(19) 0.82925(17) 0.0385(5) Uani 1 1 d .
C7 C 0.70379(16) -0.26259(19) 0.84557(16) 0.0360(4) Uani 1 1 d .
C6 C 0.75649(16) -0.08756(19) 0.89412(17) 0.0377(5) Uani 1 1 d .
C1 C 0.65274(15) -0.09256(18) 0.85674(16) 0.0348(4) Uani 1 1 d .
C3 C 0.65224(19) 0.1052(2) 0.8947(2) 0.0491(6) Uani 1 1 d .
H3A H 0.6185 0.1718 0.8964 0.059 Uiso 1 1 calc R
C2 C 0.60015(17) 0.0049(2) 0.86020(18) 0.0421(5) Uani 1 1 d .
H2A H 0.5321 0.0022 0.8399 0.051 Uiso 1 1 calc R
C10 C 0.5940(2) -0.5522(2) 0.7771(3) 0.0586(7) Uani 1 1 d D
H10B H 0.643(2) -0.590(3) 0.763(2) 0.070 Uiso 1 1 d D
H10A H 0.613(2) -0.581(3) 0.8474(16) 0.070 Uiso 1 1 d D
C5 C 0.80967(18) 0.0134(2) 0.92926(19) 0.0475(6) Uani 1 1 d .
H5A H 0.8781 0.0158 0.9526 0.057 Uiso 1 1 calc R
C4 C 0.7556(2) 0.1096(2) 0.9276(2) 0.0530(6) Uani 1 1 d .
H4A H 0.7881 0.1794 0.9487 0.064 Uiso 1 1 calc R
C9 C 0.79502(18) -0.4513(2) 0.8562(2) 0.0524(6) Uani 1 1 d .
H9A H 0.7814 -0.5315 0.8418 0.079 Uiso 1 1 calc R
H9B H 0.8369 -0.4411 0.9284 0.079 Uiso 1 1 calc R
H9C H 0.8277 -0.4219 0.8158 0.079 Uiso 1 1 calc R
C11 C 0.4967(4) -0.5872(4) 0.7079(4) 0.0515(12) Uani 0.50 1 d P
N4 N 0.47635(14) -0.25075(19) 0.94616(16) 0.0459(5) Uani 1 1 d U
O2 O 0.4155(3) -0.1816(3) 0.8973(2) 0.1065(11) Uani 1 1 d U
O1 O 0.51226(15) -0.2515(2) 1.04238(15) 0.0722(7) Uani 1 1 d U
O3 O 0.50307(14) -0.32617(15) 0.90129(14) 0.0497(4) Uani 1 1 d U
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
N3 Ni1 N3 94.79(11) 2_656 .
N3 Ni1 N2 167.81(8) 2_656 .
N3 Ni1 N2 79.51(8) . .
N3 Ni1 N2 79.51(8) 2_656 2_656
N3 Ni1 N2 167.81(8) . 2_656
N2 Ni1 N2 108.05(10) . 2_656
N3 Ni1 O3 87.46(7) 2_656 2_656
N3 Ni1 O3 84.98(8) . 2_656
N2 Ni1 O3 102.62(7) . 2_656
N2 Ni1 O3 84.02(8) 2_656 2_656
N3 Ni1 O3 84.98(8) 2_656 .
N3 Ni1 O3 87.46(7) . .
N2 Ni1 O3 84.02(8) . .
N2 Ni1 O3 102.62(7) 2_656 .
O3 Ni1 O3 168.82(9) 2_656 .
C7 N2 C1 105.57(18) . .
C7 N2 Ni1 109.65(14) . .
C1 N2 Ni1 144.59(15) . .
C7 N1 C6 107.02(18) . .
C7 N1 H1A 126.5 . .
C6 N1 H1A 126.5 . .
C8 N3 C10 121.3(2) . .
C8 N3 Ni1 115.61(15) . .
C10 N3 Ni1 122.80(17) . .
N3 C8 C7 113.25(19) . .
N3 C8 C9 128.2(2) . .
C7 C8 C9 118.5(2) . .
N2 C7 N1 113.05(19) . .
N2 C7 C8 120.62(19) . .
N1 C7 C8 126.24(19) . .
N1 C6 C5 131.7(2) . .
N1 C6 C1 105.63(19) . .
C5 C6 C1 122.7(2) . .
N2 C1 C2 131.4(2) . .
N2 C1 C6 108.70(18) . .
C2 C1 C6 119.8(2) . .
C2 C3 C4 121.5(2) . .
C2 C3 H3A 119.2 . .
C4 C3 H3A 119.2 . .
C3 C2 C1 117.7(2) . .
C3 C2 H2A 121.1 . .
C1 C2 H2A 121.1 . .
C11 C10 N3 117.4(3) . .
C11 C10 C11 46.5(4) . 2_656
N3 C10 C11 111.1(3) . 2_656
C11 C10 H10B 112(2) . .
N3 C10 H10B 113(2) . .
C11 C10 H10B 136(2) 2_656 .
C11 C10 H10A 113(2) . .
N3 C10 H10A 102(2) . .
C11 C10 H10A 69.9(19) 2_656 .
H10B C10 H10A 98(2) . .
C4 C5 C6 116.3(2) . .
C4 C5 H5A 121.8 . .
C6 C5 H5A 121.8 . .
C5 C4 C3 121.8(2) . .
C5 C4 H4A 119.1 . .
C3 C4 H4A 119.1 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C11 C10 70.4(5) 2_656 .
C11 C11 C10 63.1(5) 2_656 2_656
C10 C11 C10 122.2(4) . 2_656
O2 N4 O1 121.1(2) . .
O2 N4 O3 120.3(2) . .
O1 N4 O3 118.6(2) . .
N4 O3 Ni1 124.74(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3 2.0694(19) 2_656
Ni1 N3 2.0694(19) .
Ni1 N2 2.0736(19) .
Ni1 N2 2.0736(19) 2_656
Ni1 O3 2.1478(18) 2_656
Ni1 O3 2.1478(18) .
N2 C7 1.317(3) .
N2 C1 1.383(3) .
N1 C7 1.347(3) .
N1 C6 1.376(3) .
N1 H1A 0.8600 .
N3 C8 1.272(3) .
N3 C10 1.469(3) .
C8 C7 1.476(3) .
C8 C9 1.496(3) .
C6 C5 1.388(3) .
C6 C1 1.408(3) .
C1 C2 1.391(3) .
C3 C2 1.374(3) .
C3 C4 1.409(4) .
C3 H3A 0.9300 .
C2 H2A 0.9300 .
C10 C11 1.428(6) .
C10 C11 1.509(7) 2_656
C10 H10B 0.939(19) .
C10 H10A 0.978(18) .
C5 C4 1.374(4) .
C5 H5A 0.9300 .
C4 H4A 0.9300 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C11 C11 1.162(10) 2_656
C11 C10 1.509(7) 2_656
N4 O2 1.194(3) .
N4 O1 1.245(3) .
N4 O3 1.246(3) .
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
N1 H1A O1 0.86 1.95 2.798(3) 170.2 7_647
N1 H1A N4 0.86 2.63 3.387(3) 147.4 7_647
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
N3 Ni1 N2 C7 72.4(4) 2_656 .
N3 Ni1 N2 C7 9.56(15) . .
N2 Ni1 N2 C7 -160.57(18) 2_656 .
O3 Ni1 N2 C7 -72.82(16) 2_656 .
O3 Ni1 N2 C7 98.07(16) . .
N3 Ni1 N2 C1 -113.8(4) 2_656 .
N3 Ni1 N2 C1 -176.7(3) . .
N2 Ni1 N2 C1 13.2(2) 2_656 .
O3 Ni1 N2 C1 100.9(3) 2_656 .
O3 Ni1 N2 C1 -88.2(3) . .
N3 Ni1 N3 C8 -179.4(2) 2_656 .
N2 Ni1 N3 C8 -10.30(16) . .
N2 Ni1 N3 C8 119.1(3) 2_656 .
O3 Ni1 N3 C8 93.55(17) 2_656 .
O3 Ni1 N3 C8 -94.69(17) . .
N3 Ni1 N3 C10 6.47(17) 2_656 .
N2 Ni1 N3 C10 175.6(2) . .
N2 Ni1 N3 C10 -55.0(4) 2_656 .
O3 Ni1 N3 C10 -80.6(2) 2_656 .
O3 Ni1 N3 C10 91.2(2) . .
C10 N3 C8 C7 -177.3(2) . .
Ni1 N3 C8 C7 8.5(2) . .
C10 N3 C8 C9 1.5(4) . .
Ni1 N3 C8 C9 -172.65(19) . .
C1 N2 C7 N1 -1.7(3) . .
Ni1 N2 C7 N1 174.59(15) . .
C1 N2 C7 C8 175.09(18) . .
Ni1 N2 C7 C8 -8.7(2) . .
C6 N1 C7 N2 0.7(3) . .
C6 N1 C7 C8 -175.8(2) . .
N3 C8 C7 N2 0.4(3) . .
C9 C8 C7 N2 -178.6(2) . .
N3 C8 C7 N1 176.7(2) . .
C9 C8 C7 N1 -2.3(3) . .
C7 N1 C6 C5 -179.2(2) . .
C7 N1 C6 C1 0.6(2) . .
C7 N2 C1 C2 -175.4(2) . .
Ni1 N2 C1 C2 10.7(4) . .
C7 N2 C1 C6 2.0(2) . .
Ni1 N2 C1 C6 -171.92(19) . .
N1 C6 C1 N2 -1.6(2) . .
C5 C6 C1 N2 178.2(2) . .
N1 C6 C1 C2 176.2(2) . .
C5 C6 C1 C2 -4.1(3) . .
C4 C3 C2 C1 -1.3(4) . .
N2 C1 C2 C3 -178.9(2) . .
C6 C1 C2 C3 4.0(3) . .
C8 N3 C10 C11 -159.8(3) . .
Ni1 N3 C10 C11 14.0(4) . .
C8 N3 C10 C11 149.3(3) . 2_656
Ni1 N3 C10 C11 -36.9(4) . 2_656
N1 C6 C5 C4 -179.2(2) . .
C1 C6 C5 C4 1.1(4) . .
C6 C5 C4 C3 1.7(4) . .
C2 C3 C4 C5 -1.7(4) . .
N3 C10 C11 C11 -93.8(3) . 2_656
N3 C10 C11 C10 -56.3(5) . 2_656
C11 C10 C11 C10 37.5(5) 2_656 2_656
O2 N4 O3 Ni1 27.5(4) . .
O1 N4 O3 Ni1 -154.63(19) . .
N3 Ni1 O3 N4 -110.8(2) 2_656 .
N3 Ni1 O3 N4 154.15(19) . .
N2 Ni1 O3 N4 74.44(19) . .
N2 Ni1 O3 N4 -32.8(2) 2_656 .
O3 Ni1 O3 N4 -158.42(19) 2_656 .
