#------------------------------------------------------------------------------
#$Date: 2016-03-24 16:12:39 +0100 (jue 24 de mar de 2016) $
#$Revision: 179681 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/03/7000301.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_7000301
loop_
_publ_author_name
'Lee, Young Hoon'
'Harrowfield, Jack'
'Kim, Yang'
'Lim, Woo Taik'
'Park, Yu Cheol'
'Thuéry, Pierre'
_publ_section_title
;
 Functionalised azetidines as ligands: pyridyl-complemented
 coordination
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              434
_journal_page_last               442
_journal_paper_doi               10.1039/b812295d
_journal_year                    2009
_chemical_formula_sum            'C24 H40 Cl2 N8 Ni2 O4'
_chemical_formula_weight         692.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.5520(17)
_cell_length_b                   7.9080(16)
_cell_length_c                   21.228(4)
_cell_measurement_reflns_used    5406
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      3.09
_cell_volume                     1435.6(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       'two φ and two ω scans with 2° steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Synchrotron Radiation'
_diffrn_radiation_type           'Synchrotron Radiation'
_diffrn_radiation_wavelength     0.80000
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5186
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         30.38
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark Yellow'
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0143(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0380
_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)+(0.0692P)²+1.3864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                2736
_reflns_number_total             2834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812295d.txt
_cod_data_source_block           yk0662
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'NONE' changed to
'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P1 21/n 1'
_cod_database_code               7000301
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.37021(3) 0.26694(4) 0.050461(12) 0.00762(16) Uani 1 1 d . . .
Cl1 Cl 0.83911(7) -0.25767(7) 0.16799(3) 0.01482(18) Uani 1 1 d . . .
N1 N 0.2563(2) 0.4727(2) 0.02904(8) 0.0096(4) Uani 1 1 d . . .
N2 N 0.5045(2) 0.0927(2) 0.07376(8) 0.0099(4) Uani 1 1 d . . .
N3 N 0.3936(2) 0.3379(2) 0.13615(8) 0.0084(4) Uani 1 1 d . . .
N4 N 0.3683(2) 0.1531(3) -0.02949(8) 0.0118(4) Uani 1 1 d . . .
C1 C 0.1269(2) 0.6333(3) -0.05225(10) 0.0141(5) Uani 1 1 d . . .
C2 C 0.5408(2) -0.0182(3) 0.03019(9) 0.0100(4) Uani 1 1 d . . .
C3 C 0.4796(2) 0.5036(3) 0.13386(10) 0.0115(4) Uani 1 1 d . . .
C5 C 0.4565(3) 0.1973(3) 0.17566(10) 0.0115(4) Uani 1 1 d . . .
C6 C 0.3181(2) 0.5944(3) 0.13297(9) 0.0089(4) Uani 1 1 d . . .
C7 C 0.1898(2) 0.4848(3) -0.02895(10) 0.0123(5) Uani 1 1 d . . .
C8 C 0.2537(2) 0.6124(3) 0.06658(10) 0.0094(4) Uani 1 1 d . . .
C9 C 0.2557(2) 0.4292(3) 0.16263(10) 0.0103(4) Uani 1 1 d . . .
C10 C 0.1271(3) 0.7745(3) -0.01494(12) 0.0164(5) Uani 1 1 d . . .
C11 C 0.1890(3) 0.7639(3) 0.04545(12) 0.0140(5) Uani 1 1 d . . .
C12 C 0.5750(3) 0.1025(3) 0.13646(9) 0.0115(4) Uani 1 1 d . . .
C13 C 0.3046(3) 0.7526(3) 0.17259(13) 0.0168(5) Uani 1 1 d . . .
O1 O 0.8692(3) 0.3593(3) 0.21641(10) 0.0278(5) Uani 1 1 d . . .
O2 O 1.0413(3) 0.0849(3) 0.16782(14) 0.0419(6) Uani 1 1 d . . .
H1 H 0.155(3) 0.387(4) 0.1490(13) 0.012(6) Uiso 1 1 d . . .
H2 H 0.601(3) 0.001(4) 0.1527(12) 0.007(6) Uiso 1 1 d . . .
H3 H 0.190(3) 0.858(4) 0.0731(14) 0.016(7) Uiso 1 1 d . . .
H4 H 0.351(4) 0.731(4) 0.2132(18) 0.013(9) Uiso 1 1 d . . .
H5 H 0.184(3) 0.387(4) -0.0539(12) 0.007(6) Uiso 1 1 d . . .
H6 H 0.547(3) 0.521(4) 0.0971(13) 0.012(7) Uiso 1 1 d . . .
H7 H 0.361(3) 0.132(4) 0.1811(14) 0.018(7) Uiso 1 1 d . . .
H8 H 0.085(3) 0.870(4) -0.0297(13) 0.010(6) Uiso 1 1 d . . .
H9 H 0.531(3) 0.522(4) 0.1762(14) 0.011(7) Uiso 1 1 d . . .
H10 H 0.317(5) 0.161(5) -0.0650(18) 0.021(10) Uiso 1 1 d . . .
H11 H 0.677(3) 0.164(4) 0.1342(13) 0.016(7) Uiso 1 1 d . . .
H12 H 0.265(3) 0.437(4) 0.2087(13) 0.015(7) Uiso 1 1 d . . .
H13 H 0.359(4) 0.849(4) 0.1534(15) 0.012(7) Uiso 1 1 d . . .
H14 H 0.495(4) 0.244(4) 0.2141(17) 0.019(8) Uiso 1 1 d . . .
H15 H 0.084(4) 0.637(4) -0.0928(15) 0.012(8) Uiso 1 1 d . . .
H16 H 0.980(5) 0.157(6) 0.1882(19) 0.014(11) Uiso 1 1 d . . .
H17 H 0.201(5) 0.788(5) 0.1792(18) 0.019(10) Uiso 1 1 d . . .
H18 H 0.815(5) 0.342(6) 0.246(2) 0.017(11) Uiso 1 1 d . . .
H19 H 0.985(8) 0.005(9) 0.176(3) 0.010(2) Uiso 1 1 d . . .
H20 H 0.858(4) 0.452(6) 0.2073(17) 0.011(10) Uiso 1 1 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'
Cl Cl 0.1484 0.1585 '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
N2 Ni1 N3 84.37(8) . . ?
N2 Ni1 N4 83.76(8) . . ?
N3 Ni1 N4 167.90(8) . . ?
N2 Ni1 N1 171.16(8) . . ?
N3 Ni1 N1 91.59(8) . . ?
N4 Ni1 N1 100.50(8) . . ?
C7 N1 C8 117.77(19) . . ?
C7 N1 Ni1 118.53(15) . . ?
C8 N1 Ni1 123.33(14) . . ?
C2 N2 C12 125.43(18) . . ?
C2 N2 Ni1 117.05(14) . . ?
C12 N2 Ni1 117.09(14) . . ?
C5 N3 C9 115.62(16) . . ?
C5 N3 C3 119.47(17) . . ?
C9 N3 C3 88.71(16) . . ?
C5 N3 Ni1 110.64(13) . . ?
C9 N3 Ni1 114.78(13) . . ?
C3 N3 Ni1 105.92(12) . . ?
C2 N4 Ni1 112.65(14) 3_655 . ?
C10 C1 C7 119.1(2) . . ?
N2 C2 N4 133.50(19) . 3_655 ?
N2 C2 C2 111.6(2) . 3_655 ?
N4 C2 C2 114.9(2) 3_655 3_655 ?
N3 C3 C6 88.17(15) . . ?
N3 C5 C12 107.52(17) . . ?
C13 C6 C8 114.23(19) . . ?
C13 C6 C9 116.45(19) . . ?
C8 C6 C9 109.42(17) . . ?
C13 C6 C3 116.38(19) . . ?
C8 C6 C3 111.95(17) . . ?
C9 C6 C3 85.01(16) . . ?
N1 C7 C1 123.1(2) . . ?
N1 C8 C11 121.07(19) . . ?
N1 C8 C6 117.42(19) . . ?
C11 C8 C6 121.5(2) . . ?
N3 C9 C6 88.94(15) . . ?
C1 C10 C11 119.0(2) . . ?
C10 C11 C8 119.9(2) . . ?
N2 C12 C5 104.61(17) . . ?
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 N2 1.8600(19) . ?
Ni1 N3 1.9134(17) . ?
Ni1 N4 1.9211(19) . ?
Ni1 N1 1.9496(19) . ?
N1 C7 1.358(3) . ?
N1 C8 1.362(3) . ?
N2 C2 1.312(3) . ?
N2 C12 1.461(3) . ?
N3 C5 1.492(3) . ?
N3 C9 1.494(3) . ?
N3 C3 1.504(3) . ?
N4 C2 1.321(3) 3_655 ?
C1 C10 1.370(4) . ?
C1 C7 1.383(3) . ?
C2 N4 1.321(3) 3_655 ?
C2 C2 1.485(4) 3_655 ?
C3 C6 1.557(3) . ?
C5 C12 1.512(3) . ?
C6 C13 1.512(3) . ?
C6 C8 1.518(3) . ?
C6 C9 1.546(3) . ?
C8 C11 1.394(3) . ?
C10 C11 1.388(4) . ?
