#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:23:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180336 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/05/7200561.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_7200561
loop_
_publ_author_name
'Cao, Man-Li'
'Mo, Hao-Jun'
'Liang, Jin-Juan'
'Ye, Bao-Hui'
_publ_section_title
;
 Reversible single-crystal-to-single-crystal transformation driven by
 adsorption/desorption of water over organic solvents and thermal
 stimulation
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              784
_journal_paper_doi               10.1039/b817993j
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C26 H16 N10 Ni O2'
_chemical_formula_weight         559.18
_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                 121.308(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9760(9)
_cell_length_b                   17.636(2)
_cell_length_c                   11.0530(10)
_cell_measurement_reflns_used    2255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.31
_cell_volume                     1161.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart Apex 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4938
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.8157
_exptl_absorpt_correction_T_min  0.7529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0362
_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)+(0.0628P)²+0.2147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                1930
_reflns_number_total             2255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817993j.txt
_cod_data_source_block           complex_2a
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7200561
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 0.5000 0.5000 0.5000 0.01860(15) Uani 1 2 d S . .
O1 O 0.2600(3) 0.43286(8) 0.50294(16) 0.0243(3) Uani 1 1 d . . .
N1 N 0.7295(4) 0.41586(14) 0.0478(2) 0.0469(6) Uani 1 1 d . . .
N2 N 0.3608(3) 0.41257(9) 0.34420(19) 0.0232(4) Uani 1 1 d . . .
N3 N 0.2442(3) 0.30078(11) 0.2094(2) 0.0319(5) Uani 1 1 d . . .
N4 N 0.1216(3) 0.32436(10) 0.3706(2) 0.0276(4) Uani 1 1 d . . .
N5 N -0.2547(3) 0.07999(10) 0.1263(2) 0.0237(4) Uani 1 1 d . . .
C1 C 0.6055(5) 0.35316(17) 0.0198(3) 0.0488(7) Uani 1 1 d . . .
H1A H 0.6010 0.3193 -0.0459 0.059 Uiso 1 1 d R . .
C2 C 0.4835(5) 0.33641(14) 0.0813(3) 0.0397(6) Uani 1 1 d . . .
H2A H 0.3995 0.2920 0.0559 0.048 Uiso 1 1 d R . .
C3 C 0.4851(4) 0.38581(12) 0.1792(2) 0.0280(5) Uani 1 1 d . . .
C4 C 0.6115(4) 0.45136(13) 0.2085(3) 0.0327(5) Uani 1 1 d . . .
H4A H 0.6187 0.4863 0.2735 0.039 Uiso 1 1 d R . .
C5 C 0.7294(4) 0.46297(16) 0.1413(3) 0.0417(6) Uani 1 1 d . . .
H5A H 0.8140 0.5072 0.1643 0.050 Uiso 1 1 d R . .
C6 C 0.3561(4) 0.36629(12) 0.2479(2) 0.0253(5) Uani 1 1 d . . .
C7 C 0.2426(4) 0.38957(11) 0.4066(2) 0.0236(5) Uani 1 1 d . . .
C8 C 0.1317(4) 0.28392(12) 0.2733(2) 0.0270(5) Uani 1 1 d . . .
C9 C 0.0033(4) 0.21085(12) 0.2287(2) 0.0272(5) Uani 1 1 d . . .
C10 C 0.0117(4) 0.16604(13) 0.1295(2) 0.0310(5) Uani 1 1 d . . .
H10A H 0.1050 0.1783 0.0969 0.037 Uiso 1 1 d R . .
C11 C -0.1187(4) 0.10145(12) 0.0821(3) 0.0295(5) Uani 1 1 d . . .
H11A H -0.1109 0.0710 0.0165 0.035 Uiso 1 1 d R . .
C12 C -0.2538(5) 0.12149(14) 0.2280(3) 0.0387(6) Uani 1 1 d . . .
H12A H -0.3448 0.1067 0.2611 0.046 Uiso 1 1 d R . .
C13 C -0.1268(5) 0.18670(14) 0.2820(3) 0.0410(7) Uani 1 1 d . . .
H13A H -0.1297 0.2142 0.3523 0.049 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'
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
O1 Ni1 O1 180.00(6) . 3_666 ?
O1 Ni1 N5 89.51(7) . 4_666 ?
O1 Ni1 N5 90.49(7) 3_666 4_666 ?
O1 Ni1 N5 90.49(7) . 2 ?
O1 Ni1 N5 89.51(7) 3_666 2 ?
N5 Ni1 N5 180.0 4_666 2 ?
O1 Ni1 N2 64.23(6) . . ?
O1 Ni1 N2 115.77(6) 3_666 . ?
N5 Ni1 N2 85.57(7) 4_666 . ?
N5 Ni1 N2 94.43(7) 2 . ?
O1 Ni1 N2 115.77(6) . 3_666 ?
O1 Ni1 N2 64.23(6) 3_666 3_666 ?
N5 Ni1 N2 94.43(7) 4_666 3_666 ?
N5 Ni1 N2 85.57(7) 2 3_666 ?
N2 Ni1 N2 180.0 . 3_666 ?
O1 Ni1 C7 30.55(6) . . ?
O1 Ni1 C7 149.45(6) 3_666 . ?
N5 Ni1 C7 84.99(7) 4_666 . ?
N5 Ni1 C7 95.01(7) 2 . ?
N2 Ni1 C7 33.82(7) . . ?
N2 Ni1 C7 146.18(7) 3_666 . ?
O1 Ni1 C7 149.45(6) . 3_666 ?
O1 Ni1 C7 30.55(6) 3_666 3_666 ?
N5 Ni1 C7 95.01(7) 4_666 3_666 ?
N5 Ni1 C7 84.99(7) 2 3_666 ?
N2 Ni1 C7 146.18(7) . 3_666 ?
N2 Ni1 C7 33.82(7) 3_666 3_666 ?
C7 Ni1 C7 180.0 . 3_666 ?
C7 O1 Ni1 93.29(12) . . ?
C5 N1 C1 115.8(2) . . ?
C6 N2 C7 116.53(18) . . ?
C6 N2 Ni1 154.52(15) . . ?
C7 N2 Ni1 87.05(12) . . ?
C8 N3 C6 115.58(19) . . ?
C8 N4 C7 114.03(19) . . ?
C11 N5 C12 117.41(19) . . ?
C11 N5 Ni1 116.07(14) . 2_545 ?
C12 N5 Ni1 125.02(16) . 2_545 ?
N1 C1 C2 123.9(3) . . ?
N1 C1 H1A 117.9 . . ?
C2 C1 H1A 118.2 . . ?
C1 C2 C3 119.8(2) . . ?
C1 C2 H2A 119.2 . . ?
C3 C2 H2A 120.9 . . ?
C2 C3 C4 117.0(2) . . ?
C2 C3 C6 119.4(2) . . ?
C4 C3 C6 123.6(2) . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 H4A 120.4 . . ?
N1 C5 C4 124.6(2) . . ?
N1 C5 H5A 118.7 . . ?
C4 C5 H5A 116.6 . . ?
N2 C6 N3 123.7(2) . . ?
N2 C6 C3 119.79(19) . . ?
N3 C6 C3 116.48(19) . . ?
O1 C7 N4 122.14(19) . . ?
O1 C7 N2 114.95(18) . . ?
N4 C7 N2 122.89(19) . . ?
O1 C7 Ni1 56.16(10) . . ?
N4 C7 Ni1 172.68(17) . . ?
N2 C7 Ni1 59.13(10) . . ?
N4 C8 N3 127.2(2) . . ?
N4 C8 C9 117.09(19) . . ?
N3 C8 C9 115.68(19) . . ?
C13 C9 C10 118.1(2) . . ?
C13 C9 C8 122.5(2) . . ?
C10 C9 C8 119.33(19) . . ?
C11 C10 C9 119.0(2) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
N5 C11 C10 123.5(2) . . ?
N5 C11 H11A 117.8 . . ?
C10 C11 H11A 118.7 . . ?
N5 C12 C13 122.6(2) . . ?
N5 C12 H12A 118.5 . . ?
C13 C12 H12A 118.9 . . ?
C9 C13 C12 119.2(2) . . ?
C9 C13 H13A 120.2 . . ?
C12 C13 H13A 120.6 . . ?
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 O1 2.0644(14) . ?
Ni1 O1 2.0644(14) 3_666 ?
Ni1 N5 2.0938(17) 4_666 ?
Ni1 N5 2.0938(17) 2 ?
Ni1 N2 2.1326(17) . ?
Ni1 N2 2.1326(17) 3_666 ?
Ni1 C7 2.481(2) . ?
Ni1 C7 2.481(2) 3_666 ?
O1 C7 1.263(3) . ?
N1 C5 1.327(3) . ?
N1 C1 1.338(4) . ?
N2 C6 1.328(3) . ?
N2 C7 1.383(3) . ?
N3 C8 1.334(3) . ?
N3 C6 1.334(3) . ?
N4 C8 1.323(3) . ?
N4 C7 1.358(3) . ?
N5 C11 1.328(3) . ?
N5 C12 1.339(3) . ?
N5 Ni1 2.0938(17) 2_545 ?
C1 C2 1.369(4) . ?
C1 H1A 0.9273 . ?
C2 C3 1.385(3) . ?
C2 H2A 0.9298 . ?
C3 C4 1.386(3) . ?
C3 C6 1.489(3) . ?
C4 C5 1.380(3) . ?
C4 H4A 0.9277 . ?
C5 H5A 0.9296 . ?
C8 C9 1.499(3) . ?
C9 C13 1.382(3) . ?
C9 C10 1.377(3) . ?
C10 C11 1.380(3) . ?
C10 H10A 0.9191 . ?
C11 H11A 0.9261 . ?
C12 C13 1.383(3) . ?
C12 H12A 0.9198 . ?
C13 H13A 0.9252 . ?
