#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/21/44/7214402.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_7214402
loop_
_publ_author_name
'Ju, Zemin'
'Cao, Dapeng'
'Qin, Ling'
'Zhang, Chuanlei'
'Zhang, Mingdao'
'Shi, Zhiqiang'
'Zheng, Hegen'
_publ_section_title
;
 Syntheses, characterization, and properties of five coordination
 compounds based on the ligand tetrakis(4-pyridyloxymethylene)methane
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3917
_journal_paper_doi               10.1039/c3ce42477d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C29 H32 N4 Ni O12'
_chemical_formula_sum            'C29 H32 N4 Ni O12'
_chemical_formula_weight         687.30
_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                 108.815(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.334(2)
_cell_length_b                   9.2474(10)
_cell_length_c                   20.562(2)
_cell_measurement_temperature    291(2)
_cell_volume                     3119.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7553
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0427
_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)+(0.0743P)²+2.0244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                2482
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42477d2.cif
_cod_data_source_block           cao
_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/RSC/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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constra' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      ' C2/c'
_cod_database_code               7214402
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 0.2500 1.2500 0.5000 0.02027(17) Uani 1 2 d S
O3 O 0.22124(10) 1.38359(17) 0.41292(8) 0.0288(4) Uani 1 1 d .
O1 O 0.36015(10) 1.20160(19) 0.48606(9) 0.0306(4) Uani 1 1 d .
O2 O 0.37654(11) 0.9835(2) 0.53489(10) 0.0420(5) Uani 1 1 d .
N1 N 0.19493(12) 1.0780(2) 0.43412(10) 0.0273(4) Uani 1 1 d .
O5 O 0.02954(11) 0.35744(19) 0.18614(9) 0.0404(5) Uani 1 1 d .
C8 C 0.06726(14) 0.4602(2) 0.23894(13) 0.0311(5) Uani 1 1 d .
H8A H 0.1053 0.5200 0.2252 0.037 Uiso 1 1 calc R
H8B H 0.0969 0.4105 0.2812 0.037 Uiso 1 1 calc R
C13 C 0.39741(14) 1.0831(3) 0.50311(12) 0.0285(5) Uani 1 1 d .
C7 C 0.0000 0.5538(3) 0.2500 0.0268(7) Uani 1 2 d S
C5 C 0.12471(15) 0.8510(2) 0.34555(12) 0.0300(5) Uani 1 1 d .
C10 C 0.16171(19) 0.2568(3) 0.19616(17) 0.0427(7) Uani 1 1 d .
H10 H 0.1901 0.3272 0.2269 0.051 Uiso 1 1 calc R
O4 O 0.09228(13) 0.74585(16) 0.29870(10) 0.0370(5) Uani 1 1 d .
C6 C 0.03667(15) 0.6473(2) 0.31360(12) 0.0290(5) Uani 1 1 d .
H6A H -0.0059 0.7000 0.3245 0.035 Uiso 1 1 calc R
H6B H 0.0651 0.5872 0.3527 0.035 Uiso 1 1 calc R
C9 C 0.07754(17) 0.2579(2) 0.17089(15) 0.0334(6) Uani 1 1 d .
C1 C 0.15996(16) 0.9654(3) 0.45384(12) 0.0352(6) Uani 1 1 d .
H1 H 0.1594 0.9645 0.4989 0.042 Uiso 1 1 calc R
N2 N 0.16648(16) 0.0432(3) 0.13199(14) 0.0517(6) Uani 1 1 d .
C2 C 0.12443(16) 0.8497(3) 0.41246(13) 0.0350(6) Uani 1 1 d .
H2 H 0.1012 0.7736 0.4292 0.042 Uiso 1 1 calc R
C14 C 0.47314(16) 1.0617(3) 0.48242(15) 0.0410(7) Uani 1 1 d .
H14A H 0.4564 1.0459 0.4332 0.049 Uiso 1 1 calc R
H14B H 0.5050 1.1501 0.4922 0.049 Uiso 1 1 calc R
C11 C 0.20242(18) 0.1491(3) 0.17466(17) 0.0495(7) Uani 1 1 d .
H11 H 0.2591 0.1504 0.1911 0.059 Uiso 1 1 calc R
C4 C 0.16095(19) 0.9658(3) 0.32368(13) 0.0445(7) Uani 1 1 d .
H4 H 0.1623 0.9691 0.2788 0.053 Uiso 1 1 calc R
C15 C 0.0855(2) 0.0453(4) 0.10896(18) 0.0575(9) Uani 1 1 d .
H15 H 0.0587 -0.0283 0.0794 0.069 Uiso 1 1 calc R
C3 C 0.19482(18) 1.0742(3) 0.36886(14) 0.0409(6) Uani 1 1 d .
H3 H 0.2194 1.1504 0.3534 0.049 Uiso 1 1 calc R
C12 C 0.03878(18) 0.1492(3) 0.12606(17) 0.0515(8) Uani 1 1 d .
H12 H -0.0178 0.1465 0.1079 0.062 Uiso 1 1 calc R
O6 O 0.3484(18) 0.252(3) 0.3406(19) 0.86(3) Uani 1 1 d .
H6F H 0.3498 0.3396 0.3541 1.031 Uiso 1 1 d R
H6D H 0.3406 0.1966 0.3708 1.289 Uiso 1 1 d 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'
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
O1 Ni1 O1 180.0 . 7_576
O1 Ni1 O3 89.15(6) . .
O1 Ni1 O3 90.86(6) 7_576 .
O1 Ni1 O3 90.85(6) . 7_576
O1 Ni1 O3 89.14(6) 7_576 7_576
O3 Ni1 O3 180.00(7) . 7_576
O1 Ni1 N1 90.31(7) . 7_576
O1 Ni1 N1 89.69(7) 7_576 7_576
O3 Ni1 N1 92.17(7) . 7_576
O3 Ni1 N1 87.83(7) 7_576 7_576
O1 Ni1 N1 89.69(7) . .
O1 Ni1 N1 90.31(7) 7_576 .
O3 Ni1 N1 87.83(7) . .
O3 Ni1 N1 92.17(7) 7_576 .
N1 Ni1 N1 180.0 7_576 .
C13 O1 Ni1 124.17(15) . .
C1 N1 C3 115.5(2) . .
C1 N1 Ni1 123.41(16) . .
C3 N1 Ni1 121.11(16) . .
C9 O5 C8 117.76(19) . .
O5 C8 C7 107.77(17) . .
O5 C8 H8A 110.2 . .
C7 C8 H8A 110.2 . .
O5 C8 H8B 110.2 . .
C7 C8 H8B 110.2 . .
H8A C8 H8B 108.5 . .
O2 C13 O1 125.2(2) . .
O2 C13 C14 118.3(2) . .
O1 C13 C14 116.5(2) . .
C6 C7 C6 110.9(3) . 2
C6 C7 C8 108.78(13) . .
C6 C7 C8 108.71(13) 2 .
C6 C7 C8 108.71(13) . 2
C6 C7 C8 108.78(13) 2 2
C8 C7 C8 110.9(3) . 2
O4 C5 C2 124.6(2) . .
O4 C5 C4 116.6(2) . .
C2 C5 C4 118.7(2) . .
C11 C10 C9 118.3(3) . .
C11 C10 H10 120.9 . .
C9 C10 H10 120.9 . .
C5 O4 C6 117.30(19) . .
O4 C6 C7 107.52(17) . .
O4 C6 H6A 110.2 . .
C7 C6 H6A 110.2 . .
O4 C6 H6B 110.2 . .
C7 C6 H6B 110.2 . .
H6A C6 H6B 108.5 . .
O5 C9 C10 125.1(2) . .
O5 C9 C12 116.7(2) . .
C10 C9 C12 118.2(2) . .
N1 C1 C2 125.0(2) . .
N1 C1 H1 117.5 . .
C2 C1 H1 117.5 . .
C11 N2 C15 116.2(2) . .
C5 C2 C1 117.6(2) . .
C5 C2 H2 121.2 . .
C1 C2 H2 121.2 . .
C14 C14 C13 115.0(3) 5_676 .
C14 C14 H14A 108.5 5_676 .
C13 C14 H14A 108.5 . .
C14 C14 H14B 108.5 5_676 .
C13 C14 H14B 108.5 . .
H14A C14 H14B 107.5 . .
N2 C11 C10 124.5(3) . .
N2 C11 H11 117.7 . .
C10 C11 H11 117.7 . .
C3 C4 C5 119.0(2) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
N2 C15 C12 124.1(3) . .
N2 C15 H15 117.9 . .
C12 C15 H15 117.9 . .
N1 C3 C4 124.2(2) . .
N1 C3 H3 117.9 . .
C4 C3 H3 117.9 . .
C15 C12 C9 118.7(3) . .
C15 C12 H12 120.7 . .
C9 C12 H12 120.7 . .
H6F O6 H6D 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0690(16) .
Ni1 O1 2.0690(16) 7_576
Ni1 O3 2.0988(15) .
Ni1 O3 2.0988(15) 7_576
Ni1 N1 2.1075(19) 7_576
Ni1 N1 2.1075(19) .
O1 C13 1.263(3) .
O2 C13 1.249(3) .
N1 C1 1.332(3) .
N1 C3 1.342(3) .
O5 C9 1.344(3) .
O5 C8 1.432(3) .
C8 C7 1.527(3) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C13 C14 1.518(3) .
C7 C6 1.525(3) .
C7 C6 1.525(3) 2
C7 C8 1.527(3) 2
C5 O4 1.357(3) .
C5 C2 1.378(3) .
C5 C4 1.380(4) .
C10 C11 1.374(4) .
C10 C9 1.382(4) .
C10 H10 0.9300 .
O4 C6 1.430(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C9 C12 1.383(4) .
C1 C2 1.382(3) .
C1 H1 0.9300 .
N2 C11 1.328(4) .
N2 C15 1.330(4) .
C2 H2 0.9300 .
C14 C14 1.503(5) 5_676
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C11 H11 0.9300 .
C4 C3 1.365(4) .
C4 H4 0.9300 .
C15 C12 1.373(4) .
C15 H15 0.9300 .
C3 H3 0.9300 .
C12 H12 0.9300 .
O6 H6F 0.8500 .
O6 H6D 0.8500 .
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
O1 Ni1 O1 C13 85(12) 7_576 .
O3 Ni1 O1 C13 -149.85(19) . .
O3 Ni1 O1 C13 30.15(19) 7_576 .
N1 Ni1 O1 C13 117.98(19) 7_576 .
N1 Ni1 O1 C13 -62.02(19) . .
O1 Ni1 N1 C1 119.2(2) . .
O1 Ni1 N1 C1 -60.8(2) 7_576 .
O3 Ni1 N1 C1 -151.7(2) . .
O3 Ni1 N1 C1 28.3(2) 7_576 .
N1 Ni1 N1 C1 -51(16) 7_576 .
O1 Ni1 N1 C3 -59.3(2) . .
O1 Ni1 N1 C3 120.7(2) 7_576 .
O3 Ni1 N1 C3 29.9(2) . .
O3 Ni1 N1 C3 -150.1(2) 7_576 .
N1 Ni1 N1 C3 131(16) 7_576 .
C9 O5 C8 C7 -176.2(2) . .
Ni1 O1 C13 O2 -5.4(3) . .
Ni1 O1 C13 C14 174.11(17) . .
O5 C8 C7 C6 170.82(18) . .
O5 C8 C7 C6 -68.3(2) . 2
O5 C8 C7 C8 51.29(13) . 2
C2 C5 O4 C6 16.7(4) . .
C4 C5 O4 C6 -164.0(2) . .
C5 O4 C6 C7 172.37(19) . .
C6 C7 C6 O4 -53.54(14) 2 .
C8 C7 C6 O4 66.0(2) . .
C8 C7 C6 O4 -173.10(18) 2 .
C8 O5 C9 C10 -8.2(4) . .
C8 O5 C9 C12 172.2(2) . .
C11 C10 C9 O5 -178.7(3) . .
C11 C10 C9 C12 0.9(4) . .
C3 N1 C1 C2 -0.4(4) . .
Ni1 N1 C1 C2 -178.9(2) . .
O4 C5 C2 C1 -179.9(2) . .
C4 C5 C2 C1 0.8(4) . .
N1 C1 C2 C5 -0.4(4) . .
O2 C13 C14 C14 -14.6(5) . 5_676
O1 C13 C14 C14 165.8(3) . 5_676
C15 N2 C11 C10 0.6(5) . .
C9 C10 C11 N2 -1.4(5) . .
O4 C5 C4 C3 -179.7(3) . .
C2 C5 C4 C3 -0.4(4) . .
C11 N2 C15 C12 0.7(5) . .
C1 N1 C3 C4 0.9(4) . .
Ni1 N1 C3 C4 179.4(2) . .
C5 C4 C3 N1 -0.5(5) . .
N2 C15 C12 C9 -1.1(5) . .
O5 C9 C12 C15 179.9(3) . .
C10 C9 C12 C15 0.2(5) . .
