#------------------------------------------------------------------------------
#$Date: 2022-10-03 16:40:12 +0200 (Mon 03 de Oct de 2022) $
#$Revision: 278324 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/17/2001707.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2001707
loop_
_publ_author_name
'Lu, T.-H.'
'Lan, W.-J.'
'Chung, C.-S.'
_publ_section_title
;Structure of
 (1,4,7,10,13-Pentaazacyclopentadecane-N¹,N⁴,N¹⁰,N¹³)(perchlorato-O)nickel(II)
 perchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              961
_journal_page_last               963
_journal_paper_doi               10.1107/S0108270192011405
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         '[Ni1 (Cl1 O4) (C10 H25 N5)] (Cl1 O4)'
_chemical_formula_sum            'C10 H25 Cl2 N5 Ni O8'
_chemical_formula_weight         472.95
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 96.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.822(5)
_cell_length_b                   13.676(7)
_cell_length_c                   13.998(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(3)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      9.5
_cell_volume                     1866.8(15)
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7093
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6552
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        +-2.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.39
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.73573
_exptl_absorpt_correction_type
;
 empirical, based on \Y scan (North, Phillips & Mathews, 1968)
;
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       'Rectangular pillar'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.83(6)
_refine_diff_density_min         -0.72(6)
_refine_ls_extinction_coef       '0.53(4) (length in mm)'
_refine_ls_goodness_of_fit_obs   2.03
_refine_ls_hydrogen_treatment    refU
_refine_ls_number_parameters     265
_refine_ls_number_reflns         2534
_refine_ls_R_factor_obs          0.066
_refine_ls_shift/esd_max         0.421
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.074
_reflns_number_observed          2534
_reflns_number_total             3281
_reflns_observed_criterion       I>=2.5(I)
_cod_data_source_file            as1020.cif
_cod_data_source_block           as1020_structure_1_of_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1.0' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w = 1.0'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1866.8(14)
_cod_original_formula_sum        'C10 H25 Cl2 N5 Ni1 O8'
_cod_database_code               2001707
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ni .27621(10) .25947(7) .10217(7)
Cl(1) .3192(2) .2632(2) .35774(14)
Cl(2) .6803(3) .07706(17) .25933(17)
O(4) .3081(8) .1939(6) .4317(5)
O(1) .2231(10) .3380(7) .3709(8)
O(2) .2816(7) .2197(6) .2655(4)
O(3) .4552(8) .2994(8) .3621(6)
O(5) .6997(8) .0518(7) .3565(5)
O(6) .7833(11) .0300(8) .2128(9)
O(6D) .721(7) .076(5) .168(5)
O(7) .5499(8) .0462(7) .2151(6)
O(8) .7025(12) .1802(7) .2493(8)
N(1) .2346(12) .4032(8) .1334(13)
N(2) .4783(8) .3069(8) .1313(6)
N(3) .3189(7) .2551(7) -.0376(5)
N(4) .2709(11) .1076(6) .0913(7)
N(5) .0664(7) .2486(7) .0839(5)
C(1) .343(2) .4583(10) .1270(18)
C(2) .4786(18) .4129(13) .1502(12)
C(3) .5519(11) .2811(15) .0516(8)
C(4) .4595(11) .2982(14) -.0432(8)
C(5) .3056(15) .1536(11) -.0721(8)
C(6) .3408(19) .0809(10) .0090(9)
C(7) .1240(19) .0780(10) .0816(11)
C(8) .0339(14) .1545(13) .1245(10)
C(9) .0138(11) .3352(13) .1281(9)
C(10) .0934(17) .4222(11) .1001(10)
H(N1) .233 .396 .205
H(N2) .516 .270 .192
H(N3) .246 .298 -.074
H(N4) .321 .083 .155
H(N5) .040 .249 .011
H(1) .336 .486 .052
H(2) .337 .522 .174
H(3) .552 .448 .107
H(4) .514 .426 .226
H(5) .648 .322 .054
H(6) .580 .202 .056
H(7) .505 .266 -.105
H(8) .451 .378 -.057
H(9) .200 .140 -.105
H(10) .374 .141 -.128
H(11) .452 .080 .030
H(12) .309 .007 -.015
H(13) .086 .073 .003
H(14) .111 .008 .114
H(15) .059 .156 .203
H(16) -.076 .138 .108
H(17) -.096 .345 .105
H(18) .028 .327 .207
H(19) .058 .489 .131
H(20) .079 .429 .021
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(2) Ni N(1) 90.4(7) yes
O(2) Ni N(2) 88.4(3) yes
O(2) Ni N(3) 160.2(3) yes
O(2) Ni N(4) 80.7(3) yes
O(2) Ni N(5) 90.6(3) yes
N(1) Ni N(2) 82.6(4) yes
N(1) Ni N(3) 106.7(7) yes
N(1) Ni N(4) 164.3(6) yes
N(1) Ni N(5) 82.8(4) yes
N(2) Ni N(3) 84.1(3) yes
N(2) Ni N(4) 109.9(4) yes
N(2) Ni N(5) 165.3(4) yes
N(3) Ni N(4) 84.7(4) yes
N(3) Ni N(5) 101.3(3) yes
N(4) Ni N(5) 84.4(4) yes
O(4) Cl(1) O(1) 106.1(6) yes
O(4) Cl(1) O(2) 110.3(5) yes
O(4) Cl(1) O(3) 110.8(5) yes
O(1) Cl(1) O(2) 108.2(5) yes
O(1) Cl(1) O(3) 112.3(6) yes
O(2) Cl(1) O(3) 108.9(5) yes
O(5) Cl(2) O(6) 108.3(6) yes
O(5) Cl(2) O(7) 111.3(5) yes
O(5) Cl(2) O(8) 109.6(6) yes
O(6) Cl(2) O(7) 108.7(6) yes
O(6) Cl(2) O(8) 106.0(7) yes
O(7) Cl(2) O(8) 112.9(6) yes
N(1) C(1) C(2) 117.6(13) yes
N(2) C(2) C(1) 113.5(10) yes
N(2) C(3) C(4) 109.4(10) yes
N(3) C(4) C(3) 110.2(9) yes
N(3) C(5) C(6) 111.8(8) yes
N(4) C(6) C(5) 109.9(9) yes
N(4) C(7) C(8) 112.1(9) yes
N(5) C(8) C(7) 106.6(10) yes
N(3) C(4) H(7) 109.9(12) yes
Ni O(2) Cl(1) 139.3(4) yes
Ni N(1) C(1) 110.8(10) yes
Ni N(1) C(10) 108.5(9) yes
Ni N(2) C(2) 108.7(8) yes
Ni N(2) C(3) 109.1(7) yes
Ni N(3) C(4) 109.3(6) yes
Ni N(3) C(5) 108.6(7) yes
Ni N(4) C(6) 107.3(8) yes
Ni N(4) C(7) 107.0(8) yes
Ni N(5) C(8) 106.2(7) yes
Ni N(5) C(9) 106.9(7) yes
C(1) N(1) C(10) 130.3(16) yes
C(2) N(2) C(3) 113.0(12) yes
C(4) N(3) C(5) 113.5(10) yes
C(6) N(4) C(7) 113.9(11) yes
C(8) N(5) C(9) 116.4(11) yes
N(1) C(10) C(9) 106.9(11) yes
N(5) C(9) C(10) 108.2(10) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni O(2) 2.344(6) yes
Ni N(1) 2.063(10) yes
Ni N(2) 2.082(8) yes
Ni N(3) 2.051(8) yes
Ni N(4) 2.083(8) yes
Ni N(5) 2.051(7) yes
Cl(1) O(4) 1.418(8) yes
Cl(1) O(1) 1.419(9) yes
Cl(1) O(2) 1.430(6) yes
Cl(1) O(3) 1.419(7) yes
Cl(2) O(5) 1.394(8) yes
Cl(2) O(6) 1.421(10) yes
Cl(2) O(6D) 1.38(7) yes
Cl(2) O(7) 1.418(8) yes
Cl(2) O(8) 1.437(9) yes
N(1) C(1) 1.32(2) yes
N(1) C(10) 1.434(19) yes
N(2) C(2) 1.48(2) yes
N(2) C(3) 1.442(17) yes
N(3) C(4) 1.512(15) yes
N(3) C(5) 1.471(17) yes
N(4) C(6) 1.456(18) yes
N(4) C(7) 1.49(2) yes
N(5) C(8) 1.456(17) yes
N(5) C(9) 1.458(17) yes
C(1) C(2) 1.46(3) yes
C(3) C(4) 1.535(16) yes
C(5) C(6) 1.516(19) yes
C(7) C(8) 1.54(3) yes
C(9) C(10) 1.50(3) yes
