#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:55:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180485 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/54/7215421.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_7215421
loop_
_publ_author_name
'Sengupta, Satirtha'
'Goswami, Arijit'
'Ganguly, Sumi'
'Bala, Sukhen'
'Bhunia, Manas Kumar'
'Mondal, Raju'
_publ_section_title
;
 Influence of chloro⋯chloro interaction and π--π stacking in 3D
 supramolecular framework construction
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6136
_journal_paper_doi               10.1039/c1ce05345k
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C25 H17 Cl3 N4 Ni O6'
_chemical_formula_weight         634.49
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.1540(10)
_cell_angle_beta                 103.1460(10)
_cell_angle_gamma                104.0380(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8694(3)
_cell_length_b                   10.1833(3)
_cell_length_c                   13.5295(4)
_cell_measurement_reflns_used    3503
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.36
_cell_volume                     1278.37(7)
_computing_cell_refinement       'Bruker APEX-2'
_computing_data_collection       'Bruker APEX-2'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w 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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18784
_diffrn_reflns_theta_full        25.78
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.876687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 (Bruker, 2001), R(int)=0.0478 before correction
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0363
_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)+(0.0345P)²+0.5104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                3836
_reflns_number_total             4868
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c1ce05345k.txt
_cod_data_source_block           10sd003_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7215421
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.30678(3) 0.15180(3) 0.32435(2) 0.01680(10) Uani 1 1 d .
Cl1 Cl -0.35096(9) 0.48824(9) 0.10625(7) 0.0489(2) Uani 1 1 d .
O1S O 0.35648(18) -0.03669(18) 0.35100(14) 0.0240(4) Uani 1 1 d .
O1 O 0.21853(18) 0.30855(18) 0.28783(14) 0.0227(4) Uani 1 1 d .
N1 N 0.5141(2) 0.2714(2) 0.36946(16) 0.0204(5) Uani 1 1 d .
N1S N 0.2238(2) -0.1028(2) 0.32617(16) 0.0230(5) Uani 1 1 d .
C1 C 0.0341(3) 0.4048(3) 0.1968(2) 0.0226(6) Uani 1 1 d .
Cl2 Cl 0.17291(9) 0.75535(8) 0.07559(6) 0.0412(2) Uani 1 1 d .
N2 N 0.2850(2) 0.1615(2) 0.47472(16) 0.0193(5) Uani 1 1 d .
O2S O 0.13476(18) -0.03295(18) 0.29422(14) 0.0228(4) Uani 1 1 d .
O2 O -0.0089(2) 0.1902(2) 0.26188(16) 0.0359(5) Uani 1 1 d .
C2 C 0.1237(3) 0.5159(3) 0.1643(2) 0.0255(6) Uani 1 1 d .
Cl3 Cl 0.30541(8) 0.53196(8) 0.17631(6) 0.0401(2) Uani 1 1 d .
O3S O 0.1861(2) -0.22424(19) 0.33404(15) 0.0364(5) Uani 1 1 d .
O3 O -0.20923(19) 0.2883(2) 0.19677(15) 0.0324(5) Uani 1 1 d .
H3A H -0.1662 0.2335 0.2222 0.049 Uiso 1 1 calc R
C3 C 0.0664(3) 0.6158(3) 0.1160(2) 0.0285(7) Uani 1 1 d .
N3 N 0.3186(2) 0.1274(2) 1.17314(16) 0.0192(5) Uani 1 1 d .
C4 C -0.0787(3) 0.6066(3) 0.0996(2) 0.0326(7) Uani 1 1 d .
H4A H -0.1162 0.6741 0.0681 0.039 Uiso 1 1 calc R
C5 C -0.1678(3) 0.4988(3) 0.1293(2) 0.0311(7) Uani 1 1 d .
C6 C -0.1154(3) 0.3952(3) 0.1754(2) 0.0266(6) Uani 1 1 d .
C7 C 0.0863(3) 0.2947(3) 0.2525(2) 0.0233(6) Uani 1 1 d .
C8 C 0.5431(3) 0.4062(3) 0.3754(2) 0.0356(8) Uani 1 1 d .
H8A H 0.4676 0.4469 0.3563 0.043 Uiso 1 1 calc R
C9 C 0.6815(3) 0.4879(3) 0.4089(3) 0.0473(10) Uani 1 1 d .
H9A H 0.6978 0.5819 0.4109 0.057 Uiso 1 1 calc R
C10 C 0.7970(3) 0.4306(3) 0.4397(2) 0.0310(7) Uani 1 1 d .
C11 C 0.7660(3) 0.2903(3) 0.4325(2) 0.0226(6) Uani 1 1 d .
H11A H 0.8394 0.2470 0.4514 0.027 Uiso 1 1 calc R
C12 C 0.6259(3) 0.2154(3) 0.3971(2) 0.0226(6) Uani 1 1 d .
H12A H 0.6071 0.1211 0.3920 0.027 Uiso 1 1 calc R
C13 C 0.9440(3) 0.5179(3) 0.4770(3) 0.0398(8) Uani 1 1 d .
H13A H 0.9573 0.6092 0.4659 0.060 Uiso 1 1 calc R
C14 C 0.2333(3) 0.1271(3) 0.7794(2) 0.0226(6) Uani 1 1 d .
H14A H 0.1402 0.1115 0.7883 0.027 Uiso 1 1 calc R
C15 C 0.2534(3) 0.1423(3) 0.6757(2) 0.0201(6) Uani 1 1 d .
C16 C 0.3880(3) 0.1626(3) 0.6533(2) 0.0249(6) Uani 1 1 d .
H16A H 0.4701 0.1704 0.7054 0.030 Uiso 1 1 calc R
C17 C 0.3986(3) 0.1710(3) 0.5543(2) 0.0253(6) Uani 1 1 d .
H17A H 0.4893 0.1840 0.5413 0.030 Uiso 1 1 calc R
C18 C 0.1557(3) 0.1454(3) 0.4958(2) 0.0213(6) Uani 1 1 d .
H18A H 0.0759 0.1410 0.4426 0.026 Uiso 1 1 calc R
C19 C 0.1367(3) 0.1351(3) 0.5933(2) 0.0229(6) Uani 1 1 d .
H19A H 0.0450 0.1233 0.6043 0.027 Uiso 1 1 calc R
C20 C 0.4436(3) 0.1470(3) 1.1450(2) 0.0282(7) Uani 1 1 d .
H20A H 0.5285 0.1616 1.1956 0.034 Uiso 1 1 calc R
C21 C 0.4522(3) 0.1466(3) 1.0446(2) 0.0305(7) Uani 1 1 d .
H21A H 0.5415 0.1607 1.0292 0.037 Uiso 1 1 calc R
C22 C 0.3278(3) 0.1253(3) 0.9664(2) 0.0221(6) Uani 1 1 d .
C23 C 0.1979(3) 0.1007(3) 0.9960(2) 0.0223(6) Uani 1 1 d .
H23A H 0.1111 0.0819 0.9469 0.027 Uiso 1 1 calc R
C24 C 0.1987(3) 0.1045(3) 1.0973(2) 0.0206(6) Uani 1 1 d .
H24A H 0.1107 0.0903 1.1147 0.025 Uiso 1 1 calc R
C25 C 0.3397(3) 0.1345(3) 0.8610(2) 0.0265(6) Uani 1 1 d .
H25A H 0.4315 0.1467 0.8501 0.032 Uiso 1 1 calc 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'
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'
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 N1 94.66(8) . .
O1 Ni1 N3 88.09(8) . 1_554
N1 Ni1 N3 92.52(8) . 1_554
O1 Ni1 N2 94.03(8) . .
N1 Ni1 N2 91.01(8) . .
N3 Ni1 N2 175.72(8) 1_554 .
O1 Ni1 O1S 168.50(7) . .
N1 Ni1 O1S 96.82(8) . .
N3 Ni1 O1S 90.58(8) 1_554 .
N2 Ni1 O1S 86.60(8) . .
O1 Ni1 O2S 107.94(7) . .
N1 Ni1 O2S 157.41(8) . .
N3 Ni1 O2S 88.39(7) 1_554 .
N2 Ni1 O2S 87.42(7) . .
O1S Ni1 O2S 60.60(7) . .
N1S O1S Ni1 92.75(14) . .
C7 O1 Ni1 123.70(17) . .
C8 N1 C12 117.5(2) . .
C8 N1 Ni1 121.66(19) . .
C12 N1 Ni1 120.82(17) . .
O3S N1S O2S 122.6(2) . .
O3S N1S O1S 121.8(2) . .
O2S N1S O1S 115.5(2) . .
C2 C1 C6 118.2(2) . .
C2 C1 C7 124.4(2) . .
C6 C1 C7 117.4(2) . .
C18 N2 C17 116.9(2) . .
C18 N2 Ni1 121.68(17) . .
C17 N2 Ni1 121.11(17) . .
N1S O2S Ni1 90.96(13) . .
C3 C2 C1 120.4(3) . .
C3 C2 Cl3 116.9(2) . .
C1 C2 Cl3 122.7(2) . .
C6 O3 H3A 109.5 . .
C4 C3 C2 120.2(3) . .
C4 C3 Cl2 117.7(2) . .
C2 C3 Cl2 122.1(2) . .
C24 N3 C20 116.3(2) . .
C24 N3 Ni1 120.07(17) . 1_556
C20 N3 Ni1 123.32(18) . 1_556
C5 C4 C3 120.3(3) . .
C5 C4 H4A 119.9 . .
C3 C4 H4A 119.9 . .
C4 C5 C6 121.2(3) . .
C4 C5 Cl1 119.5(2) . .
C6 C5 Cl1 119.3(2) . .
O3 C6 C5 118.4(2) . .
O3 C6 C1 122.0(3) . .
C5 C6 C1 119.6(3) . .
O1 C7 O2 122.9(3) . .
O1 C7 C1 120.2(2) . .
O2 C7 C1 117.0(2) . .
N1 C8 C9 122.3(3) . .
N1 C8 H8A 118.9 . .
C9 C8 H8A 118.9 . .
C8 C9 C10 120.5(3) . .
C8 C9 H9A 119.8 . .
C10 C9 H9A 119.8 . .
C11 C10 C9 116.9(2) . .
C11 C10 C13 122.7(3) . .
C9 C10 C13 120.4(3) . .
C12 C11 C10 119.4(3) . .
C12 C11 H11A 120.3 . .
C10 C11 H11A 120.3 . .
N1 C12 C11 123.4(2) . .
N1 C12 H12A 118.3 . .
C11 C12 H12A 118.3 . .
C13 C13 C10 127.2(4) 2_766 .
C13 C13 H13A 116.4 2_766 .
C10 C13 H13A 116.4 . .
C25 C14 C15 124.0(2) . .
C25 C14 H14A 118.0 . .
C15 C14 H14A 118.0 . .
C19 C15 C16 116.2(2) . .
C19 C15 C14 121.0(2) . .
C16 C15 C14 122.7(2) . .
C17 C16 C15 119.8(2) . .
C17 C16 H16A 120.1 . .
C15 C16 H16A 120.1 . .
N2 C17 C16 123.7(2) . .
N2 C17 H17A 118.2 . .
C16 C17 H17A 118.2 . .
N2 C18 C19 122.6(2) . .
N2 C18 H18A 118.7 . .
C19 C18 H18A 118.7 . .
C18 C19 C15 120.7(2) . .
C18 C19 H19A 119.6 . .
C15 C19 H19A 119.6 . .
N3 C20 C21 123.3(2) . .
N3 C20 H20A 118.4 . .
C21 C20 H20A 118.4 . .
C20 C21 C22 120.2(2) . .
C20 C21 H21A 119.9 . .
C22 C21 H21A 119.9 . .
C21 C22 C23 116.2(2) . .
C21 C22 C25 119.4(2) . .
C23 C22 C25 124.3(2) . .
C24 C23 C22 120.0(2) . .
C24 C23 H23A 120.0 . .
C22 C23 H23A 120.0 . .
N3 C24 C23 124.0(2) . .
N3 C24 H24A 118.0 . .
C23 C24 H24A 118.0 . .
C14 C25 C22 126.7(3) . .
C14 C25 H25A 116.6 . .
C22 C25 H25A 116.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.0221(18) .
Ni1 N1 2.052(2) .
Ni1 N3 2.085(2) 1_554
Ni1 N2 2.095(2) .
Ni1 O1S 2.1174(18) .
Ni1 O2S 2.1601(17) .
Cl1 C5 1.738(3) .
O1S N1S 1.279(3) .
O1 C7 1.255(3) .
N1 C8 1.327(4) .
N1 C12 1.348(3) .
N1S O3S 1.218(3) .
N1S O2S 1.273(3) .
C1 C2 1.409(4) .
C1 C6 1.416(4) .
C1 C7 1.503(4) .
Cl2 C3 1.737(3) .
N2 C18 1.343(3) .
N2 C17 1.348(3) .
O2 C7 1.268(3) .
C2 C3 1.394(4) .
C2 Cl3 1.730(3) .
O3 C6 1.335(3) .
O3 H3A 0.8200 .
C3 C4 1.378(4) .
N3 C24 1.343(3) .
N3 C20 1.344(3) .
N3 Ni1 2.085(2) 1_556
C4 C5 1.366(4) .
C4 H4A 0.9300 .
C5 C6 1.392(4) .
C8 C9 1.379(4) .
C8 H8A 0.9300 .
C9 C10 1.392(4) .
C9 H9A 0.9300 .
C10 C11 1.382(4) .
C10 C13 1.469(4) .
C11 C12 1.372(3) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
C13 C13 1.282(6) 2_766
C13 H13A 0.9300 .
C14 C25 1.325(4) .
C14 C15 1.470(4) .
C14 H14A 0.9300 .
C15 C19 1.394(4) .
C15 C16 1.398(4) .
C16 C17 1.371(4) .
C16 H16A 0.9300 .
C17 H17A 0.9300 .
C18 C19 1.378(4) .
C18 H18A 0.9300 .
C19 H19A 0.9300 .
C20 C21 1.379(4) .
C20 H20A 0.9300 .
C21 C22 1.392(4) .
C21 H21A 0.9300 .
C22 C23 1.397(4) .
C22 C25 1.461(4) .
C23 C24 1.367(4) .
C23 H23A 0.9300 .
C24 H24A 0.9300 .
C25 H25A 0.9300 .
