#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311832.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_4311832
loop_
_publ_author_name
'Belli Dell'Amico, Daniela'
'Fausto Calderazzo'
'Matteo Curiardi'
'Luca Labella'
'Fabio Marchetti'
_publ_contact_author
;
      Belli Dell Amico, Daniela 
      Dipartimento di Chimica e Chimica Industriale
      Università di Pisa
      Via Risorgimento,  35
      56126  Pisa
      Italy
;
_publ_contact_author_email       belli@dcci.unipi.it
_publ_contact_author_fax         39()0502219246
_publ_contact_author_phone       39()0502219206
_publ_section_title
;
 Bis-qtpy (qtpy = 2,2':6',2'':6'',2'''-quaterpyridine) Metal Complexes,
 [M(qtpy)₂]²⁺
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5459
_journal_page_last               5465
_journal_paper_doi               10.1021/ic049595f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C40 H28 N8 Ni, 2(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C40 H36 Cl2 N8 Ni O12'
_chemical_formula_weight         950.38
_chemical_name_systematic
;
bis-(2,2':6',2'':6'',2'''-quaterpyridine)-nickel diperchlorate tetrahydrate
;
_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                 108.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.353(8)
_cell_length_b                   8.1000(16)
_cell_length_c                   22.624(6)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.103
_cell_measurement_theta_min      2.705
_cell_volume                     4232(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Ital Structures XCS'
_computing_data_reduction        Darx2000
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WINGX-1.64 (Farrugia, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.609
_diffrn_measured_fraction_theta_max 0.609
_diffrn_measurement_device_type  'Ital Structures'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            2465
_diffrn_reflns_theta_full        23.03
_diffrn_reflns_theta_max         23.03
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.98889
_exptl_absorpt_correction_T_min  0.66766
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.429
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.429
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2699
_refine_ls_wR_factor_ref         0.2784
_reflns_number_gt                1756
_reflns_number_total             1795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049595fsi20040326_074308_2.cif
_cod_data_source_block           niqtp
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C40 H36 Cl2 N8 O12 Ni'
_cod_database_code               4311832
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.0000 -0.0476(2) 0.2500 0.0645(8) Uani 1 2 d S . .
N1 N 0.0374(3) -0.2160(9) 0.3227(3) 0.070(2) Uani 1 1 d . . .
C1 C 0.0101(5) -0.2912(14) 0.3582(4) 0.089(3) Uani 1 1 d . . .
H1 H -0.0302 -0.2891 0.3459 0.107 Uiso 1 1 calc R . .
C2 C 0.0405(7) -0.3724(15) 0.4130(5) 0.101(4) Uani 1 1 d . . .
H2 H 0.0208 -0.4243 0.4370 0.121 Uiso 1 1 calc R . .
C3 C 0.0984(7) -0.3746(16) 0.4306(5) 0.114(4) Uani 1 1 d . . .
H3 H 0.1190 -0.4294 0.4670 0.137 Uiso 1 1 calc R . .
C4 C 0.1286(6) -0.2952(17) 0.3949(5) 0.103(4) Uani 1 1 d . . .
H4 H 0.1689 -0.2948 0.4072 0.124 Uiso 1 1 calc R . .
C5 C 0.0952(5) -0.2173(13) 0.3402(4) 0.077(3) Uani 1 1 d . . .
N2 N 0.0820(3) -0.0523(10) 0.2503(3) 0.071(2) Uani 1 1 d . . .
C6 C 0.1213(4) -0.1337(15) 0.2987(4) 0.084(3) Uani 1 1 d . . .
C7 C 0.1793(5) -0.1302(17) 0.3041(6) 0.106(4) Uani 1 1 d . . .
H7 H 0.2062 -0.1839 0.3370 0.127 Uiso 1 1 calc R . .
C8 C 0.1969(5) -0.047(2) 0.2605(6) 0.120(5) Uani 1 1 d . . .
H8 H 0.2360 -0.0412 0.2643 0.143 Uiso 1 1 calc R . .
C9 C 0.1563(6) 0.0293(17) 0.2111(7) 0.110(4) Uani 1 1 d . . .
H9 H 0.1675 0.0855 0.1808 0.131 Uiso 1 1 calc R . .
C10 C 0.0986(4) 0.0197(13) 0.2076(5) 0.080(3) Uani 1 1 d . . .
N3 N 0.0011(3) 0.1178(10) 0.1711(3) 0.067(2) Uani 1 1 d . . .
C11 C 0.0496(5) 0.0950(13) 0.1563(4) 0.078(3) Uani 1 1 d . . .
C12 C 0.0530(6) 0.1192(15) 0.0975(6) 0.108(4) Uani 1 1 d . . .
H12 H 0.0873 0.0984 0.0888 0.130 Uiso 1 1 calc R . .
C13 C 0.0039(7) 0.1757(18) 0.0511(5) 0.120(5) Uani 1 1 d . . .
H13 H 0.0042 0.1898 0.0104 0.143 Uiso 1 1 calc R . .
C14 C -0.0435(6) 0.2089(14) 0.0660(5) 0.096(3) Uani 1 1 d . . .
H14 H -0.0763 0.2489 0.0358 0.115 Uiso 1 1 calc R . .
C15 C -0.0444(5) 0.1853(13) 0.1247(4) 0.085(3) Uani 1 1 d . . .
N4 N -0.1471(5) 0.2126(17) 0.0967(5) 0.124(4) Uani 1 1 d . . .
C16 C -0.0961(5) 0.2421(14) 0.1428(5) 0.089(3) Uani 1 1 d . . .
C17 C -0.0903(6) 0.3225(16) 0.1971(5) 0.103(4) Uani 1 1 d . . .
H17 H -0.0541 0.3385 0.2266 0.124 Uiso 1 1 calc R . .
C18 C -0.1408(8) 0.3802(19) 0.2072(7) 0.126(5) Uani 1 1 d . . .
H18 H -0.1392 0.4361 0.2436 0.151 Uiso 1 1 calc R . .
C19 C -0.1926(8) 0.352(3) 0.1617(11) 0.157(8) Uani 1 1 d . . .
H19 H -0.2271 0.3862 0.1672 0.189 Uiso 1 1 calc R . .
C20 C -0.1928(8) 0.273(3) 0.1083(11) 0.179(10) Uani 1 1 d . . .
H20 H -0.2284 0.2602 0.0774 0.215 Uiso 1 1 calc R . .
ClA Cl 0.13807(16) 0.5938(9) 0.10945(17) 0.0745(19) Uani 0.553(11) 1 d PG A 1
O1A O 0.1269(9) 0.7598(11) 0.0954(10) 0.222(5) Uiso 0.553(11) 1 d PG A 1
O2A O 0.1865(6) 0.552(3) 0.0928(11) 0.222(5) Uiso 0.553(11) 1 d PG A 1
O3A O 0.1480(10) 0.565(3) 0.1725(3) 0.222(5) Uiso 0.553(11) 1 d PG A 1
O4A O 0.0909(6) 0.497(2) 0.0771(9) 0.222(5) Uiso 0.553(11) 1 d PG A 1
ClB Cl 0.1374(3) 0.5355(9) 0.1138(3) 0.184(8) Uani 0.447(11) 1 d PG A 2
O1B O 0.1744(13) 0.639(4) 0.0750(14) 0.222(5) Uiso 0.447(11) 1 d PG A 2
O2B O 0.1464(15) 0.665(4) 0.1595(12) 0.222(5) Uiso 0.447(11) 1 d PG A 2
O3B O 0.0822(11) 0.566(4) 0.0693(15) 0.222(5) Uiso 0.447(11) 1 d PG A 2
O4B O 0.1561(15) 0.407(3) 0.1231(15) 0.222(5) Uiso 0.447(11) 1 d PG A 2
O5A O 0.2065(11) 0.192(3) 0.0938(11) 0.144(5) Uiso 0.481(15) 1 d P B 1
O5B O 0.2265(10) 0.249(3) 0.0608(10) 0.144(5) Uiso 0.519(15) 1 d P B 2
O6A O 0.1646(10) -0.036(3) 0.0264(10) 0.177(6) Uiso 0.598(15) 1 d P C 1
O6B O 0.2147(15) 0.039(4) -0.0069(17) 0.177(6) Uiso 0.402(15) 1 d P C 2
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
_geom_angle_publ_flag
N2 Ni N2 177.8(5) . 2 ?
N2 Ni N1 100.0(3) . 2 ?
N2 Ni N1 78.5(3) 2 2 ?
N2 Ni N1 78.5(3) . . ?
N2 Ni N1 100.0(3) 2 . ?
N1 Ni N1 99.4(4) 2 . ?
N2 Ni N3 105.9(3) . 2 ?
N2 Ni N3 75.5(3) 2 2 ?
N1 Ni N3 153.9(3) 2 2 ?
N1 Ni N3 82.9(3) . 2 ?
N2 Ni N3 75.5(3) . . ?
N2 Ni N3 105.9(3) 2 . ?
N1 Ni N3 82.9(3) 2 . ?
N1 Ni N3 153.9(3) . . ?
N3 Ni N3 106.5(4) 2 . ?
C5 N1 C1 119.6(9) . . ?
C5 N1 Ni 112.9(6) . . ?
C1 N1 Ni 126.1(7) . . ?
N1 C1 C2 121.6(11) . . ?
N1 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 119.0(12) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C2 C3 C4 121.1(12) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 116.7(12) . . ?
C5 C4 H4 121.6 . . ?
C3 C4 H4 121.6 . . ?
N1 C5 C4 121.9(11) . . ?
N1 C5 C6 116.0(8) . . ?
C4 C5 C6 122.0(11) . . ?
C10 N2 C6 120.4(8) . . ?
C10 N2 Ni 122.4(7) . . ?
C6 N2 Ni 117.1(6) . . ?
N2 C6 C7 119.8(10) . . ?
N2 C6 C5 113.6(8) . . ?
C7 C6 C5 126.6(10) . . ?
C8 C7 C6 119.4(11) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.8(11) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 118.2(11) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
N2 C10 C9 122.2(11) . . ?
N2 C10 C11 113.5(8) . . ?
C9 C10 C11 124.2(10) . . ?
C11 N3 C15 115.1(7) . . ?
C11 N3 Ni 110.6(6) . . ?
C15 N3 Ni 129.5(6) . . ?
N3 C11 C12 123.5(10) . . ?
N3 C11 C10 114.1(7) . . ?
C12 C11 C10 122.0(10) . . ?
C11 C12 C13 118.3(11) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C14 C13 C12 118.8(10) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.6(12) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 N3 123.2(10) . . ?
C14 C15 C16 119.9(10) . . ?
N3 C15 C16 116.8(8) . . ?
C20 N4 C16 113.9(15) . . ?
C17 C16 N4 125.7(11) . . ?
C17 C16 C15 122.3(11) . . ?
N4 C16 C15 111.9(10) . . ?
C16 C17 C18 117.6(13) . . ?
C16 C17 H17 121.2 . . ?
C18 C17 H17 121.2 . . ?
C19 C18 C17 118.0(14) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C20 C19 C18 119.1(16) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
N4 C20 C19 125.7(17) . . ?
N4 C20 H20 117.1 . . ?
C19 C20 H20 117.1 . . ?
O4A ClA O1A 110.7 . . ?
O4A ClA O3A 107.0 . . ?
O1A ClA O3A 110.7 . . ?
O4A ClA O2A 110.7 . . ?
O1A ClA O2A 107.0 . . ?
O3A ClA O2A 110.7 . . ?
O4B ClB O3B 121.8(19) . . ?
O4B ClB O2B 125(2) . . ?
O3B ClB O2B 105.9(15) . . ?
O4B ClB O1B 108.0(17) . . ?
O3B ClB O1B 94.9(14) . . ?
O2B ClB O1B 91.5(13) . . ?
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
Ni N2 1.994(7) . ?
Ni N2 1.994(7) 2 ?
Ni N1 2.108(7) 2 ?
Ni N1 2.108(7) . ?
Ni N3 2.239(7) 2 ?
Ni N3 2.239(7) . ?
N1 C5 1.338(12) . ?
N1 C1 1.341(12) . ?
C1 C2 1.390(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.339(19) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.398(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.457(15) . ?
N2 C10 1.298(12) . ?
N2 C6 1.373(12) . ?
C6 C7 1.378(14) . ?
C7 C8 1.373(17) . ?
C7 H7 0.9300 . ?
C8 C9 1.380(18) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(15) . ?
C9 H9 0.9300 . ?
C10 C11 1.504(15) . ?
N3 C11 1.340(11) . ?
N3 C15 1.376(13) . ?
C11 C12 1.372(13) . ?
C12 C13 1.396(18) . ?
C12 H12 0.9300 . ?
C13 C14 1.329(18) . ?
C13 H13 0.9300 . ?
C14 C15 1.347(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.514(15) . ?
N4 C20 1.31(2) . ?
N4 C16 1.365(14) . ?
C16 C17 1.358(15) . ?
C17 C18 1.399(17) . ?
C17 H17 0.9300 . ?
C18 C19 1.37(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.37(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
ClA O4A 1.3890 . ?
ClA O1A 1.3890 . ?
ClA O3A 1.3891 . ?
ClA O2A 1.3891 . ?
ClB O4B 1.13(2) . ?
ClB O3B 1.42(3) . ?
ClB O2B 1.44(2) . ?
ClB O1B 1.67(3) . ?
