#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/05/7200560.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_7200560
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 H17.2 N10 Ni O2.6'
_chemical_formula_weight         569.99
_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                 120.736(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.1011(18)
_cell_length_b                   17.440(4)
_cell_length_c                   11.2157(19)
_cell_measurement_reflns_used    2317
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.34
_cell_volume                     1193.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4837
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8663
_exptl_absorpt_correction_T_min  0.8346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0410
_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)+(0.0676P)²+0.8510P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                1947
_reflns_number_total             2317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817993j.txt
_cod_data_source_block           complex_2
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C26 H17.20 N10 Ni O2.60'
_cod_database_code               7200560
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 0.02138(17) Uani 1 2 d S . .
O1 O 0.2627(3) 0.43282(10) 0.50448(19) 0.0277(4) Uani 1 1 d . . .
N1 N 0.7245(5) 0.41899(18) 0.0552(3) 0.0565(8) Uani 1 1 d . . .
N2 N 0.3603(4) 0.41288(12) 0.3460(2) 0.0284(5) Uani 1 1 d . . .
N3 N 0.2391(4) 0.30196(13) 0.2094(3) 0.0377(6) Uani 1 1 d . . .
N4 N 0.1198(4) 0.32471(12) 0.3699(2) 0.0320(5) Uani 1 1 d . . .
N5 N -0.2633(4) 0.08198(12) 0.1200(2) 0.0273(5) Uani 1 1 d . . .
C1 C 0.5985(7) 0.3564(2) 0.0237(4) 0.0583(10) Uani 1 1 d . . .
H1A H 0.5941 0.3225 -0.0419 0.070 Uiso 1 1 d R . .
C2 C 0.4763(6) 0.33886(18) 0.0832(4) 0.0483(8) Uani 1 1 d . . .
H2A H 0.3924 0.2944 0.0579 0.058 Uiso 1 1 d R . .
C3 C 0.4795(5) 0.38731(16) 0.1821(3) 0.0336(6) Uani 1 1 d . . .
C4 C 0.6067(5) 0.45260(17) 0.2147(3) 0.0398(7) Uani 1 1 d . . .
H4A H 0.6139 0.4875 0.2797 0.048 Uiso 1 1 d R . .
C5 C 0.7253(5) 0.4652(2) 0.1496(4) 0.0503(8) Uani 1 1 d . . .
H5A H 0.8099 0.5093 0.1726 0.060 Uiso 1 1 d R . .
C6 C 0.3521(4) 0.36719(15) 0.2491(3) 0.0297(6) Uani 1 1 d . . .
C7 C 0.2429(4) 0.38954(14) 0.4076(3) 0.0274(6) Uani 1 1 d . . .
C8 C 0.1274(5) 0.28496(15) 0.2721(3) 0.0308(6) Uani 1 1 d . . .
C9 C -0.0022(5) 0.21223(15) 0.2257(3) 0.0310(6) Uani 1 1 d . . .
C10 C 0.0054(5) 0.16689(16) 0.1275(3) 0.0361(7) Uani 1 1 d . . .
H10A H 0.0988 0.1792 0.0949 0.043 Uiso 1 1 d R . .
C11 C -0.1254(5) 0.10323(16) 0.0786(3) 0.0353(7) Uani 1 1 d . . .
H11A H -0.1176 0.0728 0.0130 0.042 Uiso 1 1 d R . .
C12 C -0.2648(5) 0.12426(17) 0.2192(3) 0.0442(8) Uani 1 1 d . . .
H12A H -0.3558 0.1095 0.2523 0.053 Uiso 1 1 d R . .
C13 C -0.1358(6) 0.18893(18) 0.2752(4) 0.0468(8) Uani 1 1 d . . .
H13A H -0.1387 0.2164 0.3456 0.056 Uiso 1 1 d R . .
O1W O 0.014(3) 0.5203(11) 0.037(2) 0.154(7) Uani 0.30 1 d P . .
H1WA H -0.0472 0.4772 0.0386 0.231 Uiso 0.60 1 d 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
O1 Ni1 O1 180.00(8) . 3_666 ?
O1 Ni1 N5 89.64(8) . 4_666 ?
O1 Ni1 N5 90.36(8) 3_666 4_666 ?
O1 Ni1 N5 90.36(8) . 2 ?
O1 Ni1 N5 89.64(8) 3_666 2 ?
N5 Ni1 N5 180.000(1) 4_666 2 ?
O1 Ni1 N2 64.46(8) . . ?
O1 Ni1 N2 115.54(8) 3_666 . ?
N5 Ni1 N2 85.53(9) 4_666 . ?
N5 Ni1 N2 94.47(9) 2 . ?
O1 Ni1 N2 115.54(8) . 3_666 ?
O1 Ni1 N2 64.46(8) 3_666 3_666 ?
N5 Ni1 N2 94.47(9) 4_666 3_666 ?
N5 Ni1 N2 85.53(9) 2 3_666 ?
N2 Ni1 N2 180.000(1) . 3_666 ?
O1 Ni1 C7 30.67(8) . . ?
O1 Ni1 C7 149.33(8) 3_666 . ?
N5 Ni1 C7 85.18(9) 4_666 . ?
N5 Ni1 C7 94.82(9) 2 . ?
N2 Ni1 C7 33.91(8) . . ?
N2 Ni1 C7 146.09(8) 3_666 . ?
O1 Ni1 C7 149.33(8) . 3_666 ?
O1 Ni1 C7 30.67(8) 3_666 3_666 ?
N5 Ni1 C7 94.82(9) 4_666 3_666 ?
N5 Ni1 C7 85.18(9) 2 3_666 ?
N2 Ni1 C7 146.09(8) . 3_666 ?
N2 Ni1 C7 33.91(8) 3_666 3_666 ?
C7 Ni1 C7 180.00(7) . 3_666 ?
C7 O1 Ni1 92.95(15) . . ?
C5 N1 C1 115.7(3) . . ?
C6 N2 C7 116.5(2) . . ?
C6 N2 Ni1 154.53(19) . . ?
C7 N2 Ni1 87.38(15) . . ?
C6 N3 C8 115.6(2) . . ?
C8 N4 C7 113.8(2) . . ?
C11 N5 C12 117.1(2) . . ?
C11 N5 Ni1 117.25(17) . 2_545 ?
C12 N5 Ni1 124.52(18) . 2_545 ?
N1 C1 C2 123.8(3) . . ?
C1 C2 C3 119.8(3) . . ?
C4 C3 C2 117.1(3) . . ?
C4 C3 C6 123.1(3) . . ?
C2 C3 C6 119.8(3) . . ?
C3 C4 C5 118.8(3) . . ?
N1 C5 C4 124.7(3) . . ?
N2 C6 N3 123.7(2) . . ?
N2 C6 C3 119.4(2) . . ?
N3 C6 C3 116.9(2) . . ?
O1 C7 N4 122.3(2) . . ?
O1 C7 N2 114.8(2) . . ?
N4 C7 N2 122.9(2) . . ?
O1 C7 Ni1 56.38(12) . . ?
N4 C7 Ni1 173.5(2) . . ?
N2 C7 Ni1 58.71(13) . . ?
N4 C8 N3 127.4(2) . . ?
N4 C8 C9 117.1(2) . . ?
N3 C8 C9 115.5(2) . . ?
C10 C9 C13 117.9(2) . . ?
C10 C9 C8 119.7(2) . . ?
C13 C9 C8 122.4(2) . . ?
C11 C10 C9 119.3(2) . . ?
N5 C11 C10 123.7(2) . . ?
N5 C12 C13 122.8(3) . . ?
C9 C13 C12 119.2(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 O1 2.0737(17) . ?
Ni1 O1 2.0737(17) 3_666 ?
Ni1 N5 2.090(2) 4_666 ?
Ni1 N5 2.090(2) 2 ?
Ni1 N2 2.127(2) . ?
Ni1 N2 2.127(2) 3_666 ?
Ni1 C7 2.487(3) . ?
Ni1 C7 2.487(3) 3_666 ?
O1 C7 1.270(3) . ?
N1 C5 1.328(5) . ?
N1 C1 1.340(5) . ?
N2 C6 1.324(3) . ?
N2 C7 1.389(3) . ?
N3 C6 1.331(3) . ?
N3 C8 1.335(3) . ?
N4 C8 1.321(3) . ?
N4 C7 1.358(3) . ?
N5 C11 1.333(3) . ?
N5 C12 1.339(4) . ?
N5 Ni1 2.090(2) 2_545 ?
C1 C2 1.373(5) . ?
C2 C3 1.385(4) . ?
C3 C4 1.381(4) . ?
C3 C6 1.484(4) . ?
C4 C5 1.385(4) . ?
C8 C9 1.496(4) . ?
C9 C10 1.379(4) . ?
C9 C13 1.383(4) . ?
C10 C11 1.370(4) . ?
C12 C13 1.385(4) . ?
O1W O1W 1.03(2) 3_565 ?
