#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:08:46 +0100 (vie 25 de mar de 2016) $
#$Revision: 179828 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/24/7012498.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_7012498
loop_
_publ_author_name
'Herrera, Aida M.'
'Staples, Richard J.'
'Kryatov, Sergey V.'
'Nazarenko, Alexander Y.'
'Rybak-Akimova, Elena V.'
_publ_section_title
;
 Nickel(ii) and copper(ii) complexes with pyridine-containing
 macrocycles bearing an aminopropyl pendant arm: synthesis,
 characterization, and modifications of the pendant amino
 groupElectronic supplementary information (ESI) available: colour
 versions of Figs. 4, 5 and 7. See
 http://www.rsc.org/suppdata/dt/b2/b211489e/
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              846
_journal_paper_doi               10.1039/b211489e
_journal_year                    2003
_chemical_formula_sum            'C16 H29 Cl2 N5 Ni O8'
_chemical_formula_weight         549.05
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 91.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.275(2)
_cell_length_b                   9.314(2)
_cell_length_c                   12.170(2)
_cell_measurement_reflns_used    none
_cell_measurement_temperature    293(2)
_cell_volume                     1164.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2329
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2202
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1241P)²+0.6076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                1396
_reflns_number_total             2202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211489e.txt
_cod_data_source_block           '[Ni(L2c)](ClO4)2'
_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 'PSI-SCAN' changed to
'psi-scan' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+0.6076P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+0.6076P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/M
_cod_database_code               7012498
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.78706(9) 0.7500 0.71725(7) 0.0680(4) Uani 1 d S . .
Cl1 Cl 1.18617(19) 0.7500 0.49495(17) 0.0831(6) Uani 1 d S . .
O1 O 1.0915(9) 0.7500 0.4150(9) 0.200(5) Uani 1 d S . .
O2 O 1.1360(14) 0.8384(14) 0.5797(11) 0.149(5) Uani 0.50 d P . .
O3 O 1.2943(9) 0.8262(14) 0.4519(9) 0.140(4) Uani 0.50 d P . .
O4 O 1.2224(16) 0.6235(12) 0.5314(14) 0.160(5) Uani 0.50 d P . .
Cl2 Cl 0.7001(4) 0.7500 1.0908(3) 0.1420(12) Uani 1 d S . .
O5 O 0.6971(13) 0.7500 1.1967(7) 0.222(6) Uani 1 d S . .
O6 O 0.6333(11) 0.8739(15) 1.0475(8) 0.264(5) Uani 1 d . . .
O7 O 0.8096(14) 0.7500 1.0339(12) 0.232(6) Uani 1 d S . .
C1 C 0.9862(15) 0.9025(18) 0.8404(9) 0.102(5) Uani 0.50 d PD . .
C2 C 0.8762(15) 1.0133(17) 0.8279(13) 0.113(4) Uiso 0.50 d P . .
H2A H 0.8900 1.0711 0.7638 0.080 Uiso 0.50 d PR . .
H2B H 0.8773 1.0754 0.8909 0.080 Uiso 0.50 d PR . .
N2 N 0.7539(12) 0.9401(13) 0.8153(9) 0.099(3) Uani 0.50 d P . .
H2C H 0.7423 0.9043 0.8831 0.080 Uiso 0.50 d PR . .
C3 C 0.6528(16) 1.0359(18) 0.7969(14) 0.095(5) Uiso 0.50 d P . .
H3A H 0.6659 1.0981 0.7351 0.080 Uiso 0.50 d PR . .
H3B H 0.6408 1.0937 0.8612 0.080 Uiso 0.50 d PR . .
C4 C 0.5288(18) 0.932(2) 0.7826(14) 0.106(5) Uiso 0.50 d P . .
H4A H 0.4537 0.9933 0.7871 0.080 Uiso 0.50 d PR . .
H4B H 0.5257 0.8689 0.8446 0.080 Uiso 0.50 d PR . .
C5 C 0.5093(14) 0.8394(14) 0.6896(12) 0.103(4) Uiso 0.50 d PD . .
H5A H 0.5204 0.8967 0.6249 0.080 Uiso 0.50 d PR . .
H5B H 0.4212 0.8050 0.6891 0.080 Uiso 0.50 d PR . .
C13 C 1.1018(18) 0.919(2) 0.8916(13) 0.133(6) Uani 0.50 d PD . .
H13A H 1.1296 1.0081 0.9239 0.080 Uiso 0.50 d PR . .
N3 N 0.5987(8) 0.7154(11) 0.6825(7) 0.083(4) Uani 0.50 d PD . .
C6 C 0.551(2) 0.6108(19) 0.7648(16) 0.119(7) Uiso 0.50 d PD . .
H6A H 0.4610 0.5916 0.7462 0.080 Uiso 0.50 d PR . .
H6B H 0.5532 0.6541 0.8364 0.080 Uiso 0.50 d PR . .
C7 C 0.6142(15) 0.4753(17) 0.7722(13) 0.089(4) Uiso 0.50 d P . .
H7A H 0.6060 0.4307 0.7012 0.080 Uiso 0.50 d PR . .
H7B H 0.5715 0.4138 0.8236 0.080 Uiso 0.50 d PR . .
C8 C 0.7711(15) 0.4735(18) 0.8020(11) 0.094(4) Uiso 0.50 d P . .
H8A H 0.8028 0.3774 0.8129 0.080 Uiso 0.50 d PR . .
H8B H 0.7829 0.5251 0.8697 0.080 Uiso 0.50 d PR . .
N4 N 0.8490(8) 0.5420(9) 0.7155(7) 0.074(2) Uani 0.50 d P . .
H4C H 0.8310 0.5014 0.6499 0.080 Uiso 0.50 d PR . .
C9 C 0.9920(11) 0.5376(13) 0.7394(10) 0.089(3) Uiso 0.50 d P . .
H9A H 1.0383 0.5296 0.6719 0.080 Uiso 0.50 d PR . .
H9B H 1.0122 0.4546 0.7833 0.080 Uiso 0.50 d PR . .
C10 C 1.0381(13) 0.6681(19) 0.7976(10) 0.089(4) Uani 0.50 d PD . .
C11 C 1.1563(15) 0.682(3) 0.8528(13) 0.111(7) Uani 0.50 d PD . .
H11A H 1.2123 0.5998 0.8580 0.080 Uiso 0.50 d PR . .
C12 C 1.1891(16) 0.810(3) 0.9008(13) 0.121(11) Uani 0.50 d PD . .
H12A H 1.2713 0.8181 0.9392 0.080 Uiso 0.50 d PR . .
N5 N 0.8296(9) 0.8352(10) 0.5683(7) 0.080(2) Uani 0.50 d P . .
H5C H 0.9165 0.8437 0.5631 0.080 Uiso 0.50 d PR . .
H5D H 0.7953 0.9239 0.5641 0.080 Uiso 0.50 d PR . .
C16 C 0.7772(9) 0.7500 0.4723(8) 0.090(2) Uiso 1 d S . .
H16A H 0.8093 0.6534 0.4774 0.080 Uiso 0.50 d PR . .
H16B H 0.8064 0.7908 0.4046 0.080 Uiso 0.50 d PR . .
C15 C 0.6334(9) 0.7500 0.4753(8) 0.100(3) Uiso 1 d S . .
H15A H 0.5995 0.7180 0.4054 0.080 Uiso 0.50 d PR . .
H15B H 0.6028 0.8460 0.4873 0.080 Uiso 0.50 d PR . .
C14 C 0.5793(12) 0.6483(13) 0.5704(9) 0.090(3) Uiso 0.50 d PD . .
H14A H 0.4884 0.6297 0.5580 0.080 Uiso 0.50 d PR . .
H14B H 0.6246 0.5583 0.5680 0.080 Uiso 0.50 d PR . .
N1 N 0.9582(10) 0.7814(15) 0.7940(6) 0.071(5) Uani 0.50 d PD . .
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
N1 Ni N3 164.3(3) . . ?
N1 Ni N5 99.1(4) . . ?
N3 Ni N5 95.6(4) . . ?
N1 Ni N4 82.6(4) . . ?
N3 Ni N4 98.4(4) . . ?
N5 Ni N4 106.8(4) . . ?
N1 Ni N2 76.6(5) . . ?
N3 Ni N2 95.0(4) . . ?
N5 Ni N2 102.2(4) . . ?
N4 Ni N2 146.6(4) . . ?
O4 Cl1 O1 115.8(7) . . ?
O4 Cl1 O2 112.3(10) . . ?
O1 Cl1 O2 104.7(7) . . ?
O4 Cl1 O3 110.7(9) . . ?
O1 Cl1 O3 106.8(6) . . ?
O2 Cl1 O3 105.9(8) . . ?
O5 Cl2 O7 123.8(10) . . ?
O5 Cl2 O6 110.3(5) . . ?
O7 Cl2 O6 102.2(6) . . ?
N1 C1 C13 119.5(19) . . ?
N1 C1 C2 112.7(12) . . ?
C13 C1 C2 127.8(16) . . ?
N2 C2 C1 109.4(12) . . ?
C3 N2 C2 111.4(13) . . ?
C3 N2 Ni 124.2(11) . . ?
C2 N2 Ni 107.5(9) . . ?
N2 C3 C4 102.9(14) . . ?
C5 C4 C3 123.2(15) . . ?
C4 C5 N3 116.1(14) . . ?
C1 C13 C12 122(2) . . ?
C5 N3 C6 104.9(10) . . ?
C5 N3 C14 107.7(9) . . ?
C6 N3 C14 107.2(11) . . ?
C5 N3 Ni 117.5(8) . . ?
C6 N3 Ni 107.2(10) . . ?
C14 N3 Ni 111.7(6) . . ?
C6 C7 C8 118.0(14) . . ?
N4 C8 C7 112.2(11) . . ?
C8 N4 C9 113.1(9) . . ?
C8 N4 Ni 103.3(8) . . ?
C9 N4 Ni 109.3(7) . . ?
C10 C9 N4 112.0(10) . . ?
N1 C10 C11 118.3(17) . . ?
N1 C10 C9 116.2(10) . . ?
C11 C10 C9 125.4(17) . . ?
C12 C11 C10 119.8(17) . . ?
C13 C12 C11 117.3(14) . . ?
C16 N5 Ni 114.0(6) . . ?
C15 C16 N5 109.0(7) . . ?
C16 C15 C14 112.2(7) . . ?
N3 C14 C15 111.5(9) . . ?
C1 N1 C10 122.9(13) . . ?
C1 N1 Ni 121.3(11) . . ?
C10 N1 Ni 115.7(10) . . ?
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 N1 1.998(10) . ?
Ni N3 1.999(9) . ?
Ni N5 2.034(8) . ?
Ni N4 2.039(9) . ?
Ni N2 2.166(11) . ?
Cl1 O4 1.311(12) . ?
Cl1 O1 1.364(9) . ?
Cl1 O2 1.424(10) . ?
Cl1 O3 1.426(9) . ?
Cl2 O5 1.290(9) . ?
Cl2 O7 1.332(11) . ?
Cl2 O6 1.438(11) . ?
C1 N1 1.29(2) . ?
C1 C13 1.34(2) . ?
C1 C2 1.54(2) . ?
C2 N2 1.436(19) . ?
N2 C3 1.38(2) . ?
C3 C4 1.60(2) . ?
C4 C5 1.44(2) . ?
C5 N3 1.479(12) . ?
C13 C12 1.36(3) . ?
N3 C6 1.488(15) . ?
N3 C14 1.511(12) . ?
C6 C7 1.42(2) . ?
C7 C8 1.65(2) . ?
C8 N4 1.479(16) . ?
N4 C9 1.494(14) . ?
C9 C10 1.480(18) . ?
C10 N1 1.34(2) . ?
C10 C11 1.38(2) . ?
C11 C12 1.37(2) . ?
N5 C16 1.504(11) . ?
C16 C15 1.479(12) . ?
C15 C14 1.603(13) . ?
