#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:39:16 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179929 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/24/7022405.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_7022405
loop_
_publ_author_name
'Massoud, Salah S.'
'Louka, Febee R.'
'Obaid, Yasser K.'
'Vicente, Ramon'
'Ribas, Joan'
'Fischer, Roland C.'
'Mautner, Franz A.'
_publ_section_title
;
 Metal ions directing the geometry and nuclearity of azido-metal(II)
 complexes derived from bis(2-(3,5-dimethyl-1H-pyrazol-1-yl)ethyl)amine.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3968
_journal_page_last               3978
_journal_paper_doi               10.1039/c2dt32540c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         '2(C28 H46 N22 Ni2), 3(H2 O)'
_chemical_formula_sum            'C56 H98 N44 Ni4 O3'
_chemical_formula_weight         1670.54
_chemical_name_common            '[Ni(dedmpza)(N3)2]2.3/2H2O)'
_chemical_name_systematic
;
?
;
_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                 92.25(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.732(3)
_cell_length_b                   10.5610(13)
_cell_length_c                   15.831(2)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     3630.6(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ω-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  0.1089
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12846
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0575
_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)+(0.0688P)²+8.6740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                3316
_reflns_number_total             3685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32540c.txt
_cod_data_source_block           s2246b
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7022405
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
Ni1 Ni 0.189912(18) 0.26514(4) 0.06244(2) 0.01450(16) Uani 1 1 d .
N1 N 0.09750(14) 0.2234(3) 0.03341(18) 0.0209(6) Uani 1 1 d .
N2 N 0.06694(13) 0.1386(3) 0.08058(17) 0.0206(6) Uani 1 1 d .
N3 N 0.20895(13) 0.0758(2) 0.09948(16) 0.0170(6) Uani 1 1 d D
H3 H 0.2330(18) 0.063(5) 0.055(2) 0.048(14) Uiso 1 1 d D
N4 N 0.20231(14) 0.2420(2) 0.25253(17) 0.0176(6) Uani 1 1 d .
N5 N 0.16975(13) 0.3011(3) 0.18858(16) 0.0171(5) Uani 1 1 d .
N11 N 0.28778(13) 0.2856(3) 0.06229(16) 0.0171(6) Uani 1 1 d .
N12 N 0.31801(13) 0.3506(3) 0.10896(16) 0.0198(6) Uani 1 1 d .
N13 N 0.34696(16) 0.4094(3) 0.1571(2) 0.0349(8) Uani 1 1 d .
N21 N 0.19000(13) 0.4547(3) 0.02644(17) 0.0216(6) Uani 1 1 d .
N22 N 0.16704(13) 0.5480(3) 0.05222(17) 0.0196(6) Uani 1 1 d .
N23 N 0.14546(15) 0.6408(3) 0.0752(2) 0.0313(7) Uani 1 1 d .
C1 C 0.05409(16) 0.2834(3) -0.0124(2) 0.0236(7) Uani 1 1 d .
C2 C -0.00370(18) 0.2381(3) 0.0067(2) 0.0284(8) Uani 1 1 d .
H2 H -0.0423 0.2661 -0.0165 0.034 Uiso 1 1 calc R
C3 C 0.00596(16) 0.1455(3) 0.0655(2) 0.0255(7) Uani 1 1 d .
C4 C -0.03774(17) 0.0630(4) 0.1091(3) 0.0336(9) Uani 1 1 d .
H4A H -0.0326 -0.0247 0.0904 0.050 Uiso 1 1 calc R
H4B H -0.0800 0.0909 0.0954 0.050 Uiso 1 1 calc R
H4C H -0.0295 0.0682 0.1703 0.050 Uiso 1 1 calc R
C5 C 0.06801(18) 0.3857(4) -0.0732(2) 0.0321(8) Uani 1 1 d .
H5A H 0.0598 0.4681 -0.0475 0.048 Uiso 1 1 calc R
H5B H 0.0420 0.3755 -0.1247 0.048 Uiso 1 1 calc R
H5C H 0.1114 0.3809 -0.0874 0.048 Uiso 1 1 calc R
C6 C 0.09972(16) 0.0409(3) 0.1293(2) 0.0231(7) Uani 1 1 d .
H6A H 0.0715 -0.0306 0.1391 0.028 Uiso 1 1 calc R
H6B H 0.1133 0.0758 0.1850 0.028 Uiso 1 1 calc R
C7 C 0.15521(16) -0.0070(3) 0.0839(2) 0.0225(7) Uani 1 1 d .
H7A H 0.1654 -0.0937 0.1036 0.027 Uiso 1 1 calc R
H7B H 0.1452 -0.0109 0.0224 0.027 Uiso 1 1 calc R
C8 C 0.23821(16) 0.0490(3) 0.1836(2) 0.0216(7) Uani 1 1 d .
H8A H 0.2760 -0.0013 0.1756 0.026 Uiso 1 1 calc R
H8B H 0.2098 -0.0039 0.2159 0.026 Uiso 1 1 calc R
C9 C 0.25515(16) 0.1644(3) 0.2357(2) 0.0212(7) Uani 1 1 d .
H9A H 0.2750 0.1370 0.2900 0.025 Uiso 1 1 calc R
H9B H 0.2854 0.2156 0.2053 0.025 Uiso 1 1 calc R
C10 C 0.20343(18) 0.2083(4) 0.4073(2) 0.0266(8) Uani 1 1 d .
H10A H 0.2057 0.1158 0.4043 0.040 Uiso 1 1 calc R
H10B H 0.1776 0.2330 0.4539 0.040 Uiso 1 1 calc R
H10C H 0.2449 0.2431 0.4170 0.040 Uiso 1 1 calc R
C11 C 0.17619(17) 0.2587(3) 0.3263(2) 0.0193(7) Uani 1 1 d .
C12 C 0.12474(16) 0.3296(3) 0.3110(2) 0.0210(7) Uani 1 1 d .
H12 H 0.0964 0.3570 0.3514 0.025 Uiso 1 1 calc R
C13 C 0.12185(15) 0.3538(3) 0.2249(2) 0.0195(7) Uani 1 1 d .
C14 C 0.07233(16) 0.4234(3) 0.1780(2) 0.0246(7) Uani 1 1 d .
H14A H 0.0851 0.4409 0.1205 0.037 Uiso 1 1 calc R
H14B H 0.0643 0.5034 0.2069 0.037 Uiso 1 1 calc R
H14C H 0.0348 0.3720 0.1756 0.037 Uiso 1 1 calc R
O1 O 0.0648(4) 0.7683(7) 0.2183(5) 0.102(2) Uani 0.75 1 d PD
H20 H 0.072(2) 0.730(12) 0.175(5) 0.153 Uiso 0.75 1 d PD
H21 H 0.0972(16) 0.791(12) 0.242(5) 0.153 Uiso 0.75 1 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'
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
N21 Ni1 N1 98.84(11) . .
N21 Ni1 N5 95.11(11) . .
N1 Ni1 N5 90.73(11) . .
N21 Ni1 N3 168.71(11) . .
N1 Ni1 N3 92.14(11) . .
N5 Ni1 N3 87.32(10) . .
N21 Ni1 N11 89.15(11) . 7
N1 Ni1 N11 89.70(11) . 7
N5 Ni1 N11 175.60(10) . 7
N3 Ni1 N11 88.29(10) . 7
N21 Ni1 N11 83.75(11) . .
N1 Ni1 N11 165.62(11) . .
N5 Ni1 N11 103.18(11) . .
N3 Ni1 N11 84.96(11) . .
N11 Ni1 N11 76.15(12) 7 .
C1 N1 N2 105.2(3) . .
C1 N1 Ni1 132.5(2) . .
N2 N1 Ni1 120.3(2) . .
C3 N2 N1 111.6(3) . .
C3 N2 C6 126.3(3) . .
N1 N2 C6 121.3(3) . .
C7 N3 C8 110.3(2) . .
C7 N3 Ni1 111.7(2) . .
C8 N3 Ni1 120.1(2) . .
C11 N4 N5 111.4(3) . .
C11 N4 C9 127.4(3) . .
N5 N4 C9 121.1(3) . .
C13 N5 N4 105.2(3) . .
C13 N5 Ni1 133.2(2) . .
N4 N5 Ni1 120.2(2) . .
N12 N11 Ni1 125.7(2) . 7
N12 N11 Ni1 125.7(2) . .
Ni1 N11 Ni1 103.85(12) 7 .
N13 N12 N11 176.7(3) . .
N22 N21 Ni1 134.5(2) . .
N23 N22 N21 177.8(3) . .
N1 C1 C2 110.2(3) . .
N1 C1 C5 122.8(3) . .
C2 C1 C5 127.0(3) . .
C3 C2 C1 106.3(3) . .
C3 C2 H2 126.8 . .
C1 C2 H2 126.8 . .
N2 C3 C2 106.6(3) . .
N2 C3 C4 122.3(3) . .
C2 C3 C4 131.1(4) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C1 C5 H5A 109.5 . .
C1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N2 C6 C7 111.6(3) . .
N2 C6 H6A 109.3 . .
C7 C6 H6A 109.3 . .
N2 C6 H6B 109.3 . .
C7 C6 H6B 109.3 . .
H6A C6 H6B 108.0 . .
N3 C7 C6 111.3(3) . .
N3 C7 H7A 109.4 . .
C6 C7 H7A 109.4 . .
N3 C7 H7B 109.4 . .
C6 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
N3 C8 C9 115.1(3) . .
N3 C8 H8A 108.5 . .
C9 C8 H8A 108.5 . .
N3 C8 H8B 108.5 . .
C9 C8 H8B 108.5 . .
H8A C8 H8B 107.5 . .
N4 C9 C8 112.4(3) . .
N4 C9 H9A 109.1 . .
C8 C9 H9A 109.1 . .
N4 C9 H9B 109.1 . .
C8 C9 H9B 109.1 . .
H9A C9 H9B 107.9 . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N4 C11 C12 107.1(3) . .
N4 C11 C10 122.7(3) . .
C12 C11 C10 130.2(3) . .
C11 C12 C13 106.4(3) . .
C11 C12 H12 126.8 . .
C13 C12 H12 126.8 . .
N5 C13 C12 110.0(3) . .
N5 C13 C14 123.8(3) . .
C12 C13 C14 126.2(3) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N21 2.082(3) .
Ni1 N1 2.090(3) .
Ni1 N5 2.096(3) .
Ni1 N3 2.120(3) .
Ni1 N11 2.120(3) 7
Ni1 N11 2.138(3) .
N1 C1 1.328(5) .
N1 N2 1.356(4) .
N2 C3 1.339(5) .
N2 C6 1.457(4) .
N3 C7 1.472(4) .
N3 C8 1.480(4) .
N4 C11 1.330(4) .
N4 N5 1.364(4) .
N4 C9 1.444(4) .
N5 C13 1.331(4) .
N11 N12 1.188(4) .
N11 Ni1 2.120(3) 7
N12 N13 1.151(4) .
N21 N22 1.184(4) .
N22 N23 1.152(4) .
C1 C2 1.389(5) .
C1 C5 1.485(5) .
C2 C3 1.360(5) .
C2 H2 0.9500 .
C3 C4 1.479(5) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.514(5) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.509(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.489(5) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.359(5) .
C12 C13 1.386(5) .
C12 H12 0.9500 .
C13 C14 1.479(5) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C1 N1 N2 C3 -0.5(4)
C1 N1 N2 C6 170.0(3)
C11 N4 N5 C13 -0.9(4)
C9 N4 N5 C13 174.6(3)
N2 N1 C1 C2 1.0(4)
N2 N1 C1 C5 179.7(3)
N1 C1 C2 C3 -1.1(4)
C5 C1 C2 C3 -179.8(3)
N1 N2 C3 C2 -0.2(4)
C6 N2 C3 C2 -170.1(3)
N1 N2 C3 C4 -179.9(3)
C6 N2 C3 C4 10.2(5)
C1 C2 C3 N2 0.8(4)
C1 C2 C3 C4 -179.6(4)
C3 N2 C6 C7 133.6(3)
N1 N2 C6 C7 -35.4(4)
C8 N3 C7 C6 79.0(3)
N2 C6 C7 N3 83.5(3)
C7 N3 C8 C9 -134.8(3)
C11 N4 C9 C8 110.1(4)
N5 N4 C9 C8 -64.5(4)
N3 C8 C9 N4 59.9(4)
N5 N4 C11 C12 0.6(4)
C9 N4 C11 C12 -174.5(3)
N5 N4 C11 C10 -177.7(3)
C9 N4 C11 C10 7.3(5)
N4 C11 C12 C13 -0.1(4)
C10 C11 C12 C13 178.0(3)
N4 N5 C13 C12 0.8(4)
N4 N5 C13 C14 -177.1(3)
C11 C12 C13 N5 -0.5(4)
C11 C12 C13 C14 177.3(3)
