#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:36:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180441 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/10/7211074.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_7211074
loop_
_publ_author_name
'Gee, William J.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Batten, Stuart R.'
_publ_section_title
;
 Coordination polymers of a dipyridylazacrown ligand: structural, thermal
 and spectroscopic properties
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9655
_journal_paper_doi               10.1039/c3ce41202d
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C48 H78 N8 Ni O10, 4(Cl O4), O, 3(H2 O)'
_chemical_formula_sum            'C48 H84 Cl4 N8 Ni O30'
_chemical_formula_weight         1453.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.43(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.576(4)
_cell_length_b                   14.207(3)
_cell_length_c                   25.869(5)
_cell_measurement_reflns_used    58514
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      1.16
_cell_volume                     6431(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Australian synchrotron MX1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1551
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58514
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.60
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            olive-green
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         16085
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1746
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0978P)²+20.7792P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2742
_reflns_number_gt                8461
_reflns_number_total             16085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41202d.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7211074
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.74690(4) 0.61139(5) 0.75723(3) 0.0322(9) Uani 1 1 d .
Cl3 Cl 0.67793(10) 0.31860(13) 0.86843(7) 0.0506(9) Uani 1 1 d .
Cl4 Cl 0.79558(10) 0.35816(12) 0.56509(7) 0.0499(9) Uani 1 1 d .
Cl1 Cl 0.83193(10) 0.94005(12) 0.83345(7) 0.0459(9) Uani 1 1 d .
Cl2 Cl 0.67326(9) 0.92912(11) 0.65328(7) 0.0459(9) Uani 1 1 d .
O2 O 0.7416(3) 0.7595(3) 0.75756(17) 0.0414(13) Uani 1 1 d D
N5 N 0.8256(3) 0.6063(4) 0.7005(2) 0.0362(14) Uani 1 1 d .
N3 N 0.6563(3) 0.6111(3) 0.69837(19) 0.0338(13) Uani 1 1 d .
N7 N 0.8404(3) 0.6180(4) 0.8145(2) 0.0371(14) Uani 1 1 d .
O1 O 0.7470(3) 0.4639(3) 0.76019(18) 0.0438(13) Uani 1 1 d D
N1 N 0.6659(3) 0.6088(4) 0.81263(19) 0.0345(13) Uani 1 1 d .
C3 C 0.5554(3) 0.5983(4) 0.8844(2) 0.0372(15) Uani 1 1 d .
O11 O 0.7880(3) 0.8591(3) 0.84812(19) 0.0462(14) Uani 1 1 d .
C28 C 0.8687(4) 0.6599(4) 0.6207(2) 0.0381(16) Uani 1 1 d .
H28 H 0.8625 0.7024 0.5922 0.046 Uiso 1 1 calc R
C5 C 0.6685(3) 0.6657(4) 0.8540(2) 0.0356(15) Uani 1 1 d .
H5 H 0.7089 0.7103 0.8587 0.043 Uiso 1 1 calc R
C27 C 0.9275(4) 0.5947(4) 0.6238(3) 0.0416(17) Uani 1 1 d .
C39 C 0.9727(4) 0.6216(4) 0.8845(3) 0.0414(16) Uani 1 1 d .
O15 O 0.7278(3) 0.8535(4) 0.6647(2) 0.0568(16) Uani 1 1 d .
C29 C 0.8189(3) 0.6633(4) 0.6588(2) 0.0356(15) Uani 1 1 d .
H29 H 0.7783 0.7077 0.6555 0.043 Uiso 1 1 calc R
O25 O 0.7315(4) 0.4005(5) 0.5850(3) 0.081(2) Uani 1 1 d .
C15 C 0.5381(3) 0.6769(4) 0.6618(2) 0.0357(15) Uani 1 1 d .
H15 H 0.5010 0.7255 0.6622 0.043 Uiso 1 1 calc R
C18 C 0.6482(3) 0.5423(4) 0.6623(2) 0.0341(15) Uani 1 1 d .
H18 H 0.6872 0.4961 0.6620 0.041 Uiso 1 1 calc R
C4 C 0.6151(3) 0.6629(4) 0.8906(2) 0.0345(15) Uani 1 1 d .
H4 H 0.6194 0.7047 0.9194 0.041 Uiso 1 1 calc R
C2 C 0.5525(4) 0.5410(4) 0.8406(3) 0.0415(16) Uani 1 1 d .
H2 H 0.5126 0.4961 0.8344 0.050 Uiso 1 1 calc R
C14 C 0.6014(3) 0.6776(4) 0.6971(2) 0.0359(15) Uani 1 1 d .
H14 H 0.6068 0.7273 0.7217 0.043 Uiso 1 1 calc R
O13 O 0.8273(4) 1.0130(4) 0.8703(3) 0.079(2) Uani 1 1 d .
C38 C 0.9566(4) 0.6919(5) 0.8475(3) 0.0445(17) Uani 1 1 d .
H38 H 0.9907 0.7435 0.8460 0.053 Uiso 1 1 calc R
O16 O 0.6002(3) 0.9019(4) 0.6665(3) 0.076(2) Uani 1 1 d .
C40 C 0.9188(4) 0.5498(4) 0.8854(3) 0.0413(16) Uani 1 1 d .
H40 H 0.9266 0.5001 0.9099 0.050 Uiso 1 1 calc R
O18 O 0.7003(4) 1.0127(4) 0.6783(3) 0.083(2) Uani 1 1 d .
C1 C 0.6069(4) 0.5491(4) 0.8062(3) 0.0432(17) Uani 1 1 d .
H1 H 0.6025 0.5102 0.7762 0.052 Uiso 1 1 calc R
C41 C 0.8543(4) 0.5511(4) 0.8507(3) 0.0408(16) Uani 1 1 d .
H41 H 0.8178 0.5022 0.8526 0.049 Uiso 1 1 calc R
C26 C 0.9338(4) 0.5370(5) 0.6668(3) 0.0489(19) Uani 1 1 d .
H26 H 0.9730 0.4909 0.6706 0.059 Uiso 1 1 calc R
O26 O 0.8371(4) 0.3038(5) 0.6046(2) 0.087(2) Uani 1 1 d .
C25 C 0.8832(4) 0.5457(5) 0.7050(3) 0.0477(18) Uani 1 1 d .
H25 H 0.8903 0.5071 0.7350 0.057 Uiso 1 1 calc R
O17 O 0.6701(4) 0.9458(4) 0.5975(2) 0.0678(18) Uani 1 1 d .
C17 C 0.5860(4) 0.5360(4) 0.6262(2) 0.0373(15) Uani 1 1 d .
H17 H 0.5820 0.4856 0.6019 0.045 Uiso 1 1 calc R
C37 C 0.8922(4) 0.6876(5) 0.8131(3) 0.0428(17) Uani 1 1 d .
H37 H 0.8838 0.7354 0.7875 0.051 Uiso 1 1 calc R
O12 O 0.9081(3) 0.9138(4) 0.8297(3) 0.079(2) Uani 1 1 d .
O20 O 0.6551(6) 0.3319(7) 0.8157(3) 0.126(3) Uani 1 1 d .
O14 O 0.7958(5) 0.9731(6) 0.7845(3) 0.094(2) Uani 1 1 d .
O23 O 0.7721(4) 0.2990(5) 0.5221(2) 0.0745(19) Uani 1 1 d .
O21 O 0.6124(5) 0.3254(5) 0.8939(4) 0.116(3) Uani 1 1 d .
O22 O 0.7117(4) 0.2292(5) 0.8766(4) 0.118(4) Uani 1 1 d .
N4 N 0.4029(3) 0.5286(4) 0.5929(2) 0.0382(14) Uani 1 1 d .
N6 N 1.0018(4) 0.6700(4) 0.5570(2) 0.0498(17) Uani 1 1 d .
N2 N 0.4671(3) 0.6728(3) 0.9431(2) 0.0374(14) Uani 1 1 d .
C6 C 0.4990(4) 0.5850(4) 0.9244(3) 0.0388(16) Uani 1 1 d .
H6A H 0.4564 0.5451 0.9091 0.047 Uiso 1 1 calc R
H6B H 0.5246 0.5506 0.9545 0.047 Uiso 1 1 calc R
C19 C 0.4608(4) 0.6045(5) 0.5849(2) 0.0395(15) Uani 1 1 d .
H19A H 0.4793 0.5962 0.5502 0.047 Uiso 1 1 calc R
H19B H 0.4352 0.6665 0.5853 0.047 Uiso 1 1 calc R
C16 C 0.5282(4) 0.6043(4) 0.6251(2) 0.0371(15) Uani 1 1 d .
C30 C 0.9785(4) 0.5811(5) 0.5803(3) 0.052(2) Uani 1 1 d .
H30A H 1.0249 0.5464 0.5940 0.062 Uiso 1 1 calc R
H30B H 0.9512 0.5419 0.5528 0.062 Uiso 1 1 calc R
C42 C 1.0424(4) 0.6267(5) 0.9221(3) 0.0483(18) Uani 1 1 d .
H42A H 1.0278 0.6144 0.9575 0.058 Uiso 1 1 calc R
H42B H 1.0638 0.6911 0.9216 0.058 Uiso 1 1 calc R
N8 N 1.1034(4) 0.5566(4) 0.9099(3) 0.067(2) Uani 1 1 d .
H8 H 1.0860 0.4964 0.9166 0.080 Uiso 1 1 calc R
C11 C 0.3896(4) 0.7069(5) 0.8594(3) 0.0450(17) Uani 1 1 d .
H11A H 0.4056 0.6480 0.8430 0.054 Uiso 1 1 calc R
H11B H 0.3373 0.7228 0.8443 0.054 Uiso 1 1 calc R
C10 C 0.3910(4) 0.6941(5) 0.9177(3) 0.0420(16) Uani 1 1 d .
H10A H 0.3718 0.7523 0.9330 0.050 Uiso 1 1 calc R
H10B H 0.3557 0.6423 0.9248 0.050 Uiso 1 1 calc R
C43 C 1.1198(5) 0.5616(6) 0.8502(4) 0.078(3) Uani 1 1 d .
H43A H 1.0833 0.6059 0.8317 0.094 Uiso 1 1 calc R
H43B H 1.1720 0.5865 0.8479 0.094 Uiso 1 1 calc R
C31 C 0.9891(6) 0.6657(5) 0.4995(3) 0.070(3) Uani 1 1 d .
H31A H 1.0227 0.7126 0.4848 0.084 Uiso 1 1 calc R
H31B H 1.0046 0.6027 0.4879 0.084 Uiso 1 1 calc R
O24 O 0.8425(4) 0.4300(6) 0.5476(3) 0.090(2) Uani 1 1 d .
O19 O 0.7283(5) 0.3919(6) 0.8806(5) 0.142(4) Uani 1 1 d .
O28 O 0.4875(3) 0.3812(3) 0.56551(17) 0.0417(13) Uani 1 1 d .
O6 O 0.3180(3) 0.3732(3) 0.52688(17) 0.0442(13) Uani 1 1 d .
O5 O 0.4668(3) 0.4258(3) 0.68369(18) 0.0449(13) Uani 1 1 d .
O4 O 0.4414(3) 0.7817(3) 0.84998(18) 0.0449(13) Uani 1 1 d .
O3 O 0.5701(3) 0.7697(3) 1.02054(17) 0.0439(13) Uani 1 1 d .
O9 O 1.0373(4) 0.4443(4) 0.8198(3) 0.0715(19) Uani 1 1 d .
O8 O 1.0372(3) 0.7887(4) 0.6444(2) 0.0557(15) Uani 1 1 d .
C22 C 0.3381(4) 0.5401(5) 0.5503(3) 0.0413(16) Uani 1 1 d .
H22A H 0.3082 0.5968 0.5576 0.050 Uiso 1 1 calc R
H22B H 0.3599 0.5504 0.5169 0.050 Uiso 1 1 calc R
O10 O 1.1568(4) 0.4627(5) 1.0104(2) 0.0698(18) Uani 1 1 d .
O7 O 0.8856(4) 0.7729(4) 0.4931(2) 0.0675(18) Uani 1 1 d .
C8 C 0.5393(4) 0.6797(5) 1.0303(3) 0.0468(18) Uani 1 1 d .
H8A H 0.5337 0.6726 1.0678 0.056 Uiso 1 1 calc R
H8B H 0.5741 0.6298 1.0199 0.056 Uiso 1 1 calc R
C13 C 0.5136(5) 0.8442(5) 0.7864(3) 0.0500(19) Uani 1 1 d .
H13A H 0.5531 0.7953 0.7943 0.060 Uiso 1 1 calc R
H13B H 0.5126 0.8598 0.7490 0.060 Uiso 1 1 calc R
C7 C 0.4621(4) 0.6701(5) 0.9995(3) 0.0447(17) Uani 1 1 d .
H7A H 0.4385 0.6098 1.0086 0.054 Uiso 1 1 calc R
H7B H 0.4285 0.7217 1.0092 0.054 Uiso 1 1 calc R
C20 C 0.3746(4) 0.5323(5) 0.6465(3) 0.0426(16) Uani 1 1 d .
H20A H 0.4007 0.5843 0.6665 0.051 Uiso 1 1 calc R
H20B H 0.3191 0.5460 0.6429 0.051 Uiso 1 1 calc R
C21 C 0.3882(4) 0.4433(6) 0.6756(3) 0.053(2) Uani 1 1 d .
H21A H 0.3664 0.4479 0.7094 0.064 Uiso 1 1 calc R
H21B H 0.3626 0.3908 0.6557 0.064 Uiso 1 1 calc R
C23 C 0.2850(4) 0.4565(5) 0.5449(3) 0.0451(17) Uani 1 1 d .
H23A H 0.2664 0.4435 0.5791 0.054 Uiso 1 1 calc R
H23B H 0.2401 0.4732 0.5206 0.054 Uiso 1 1 calc R
C12 C 0.4391(4) 0.8070(5) 0.7970(3) 0.0495(18) Uani 1 1 d .
H12A H 0.3992 0.8553 0.7888 0.059 Uiso 1 1 calc R
H12B H 0.4263 0.7512 0.7750 0.059 Uiso 1 1 calc R
C32 C 0.9100(6) 0.6835(6) 0.4784(3) 0.067(2) Uani 1 1 d .
H32A H 0.9063 0.6794 0.4400 0.081 Uiso 1 1 calc R
H32B H 0.8761 0.6347 0.4912 0.081 Uiso 1 1 calc R
C34 C 1.0785(4) 0.6973(6) 0.5752(4) 0.062(2) Uani 1 1 d .
H34A H 1.0918 0.7553 0.5568 0.075 Uiso 1 1 calc R
H34B H 1.1141 0.6472 0.5663 0.075 Uiso 1 1 calc R
C35 C 1.0899(4) 0.7151(6) 0.6331(4) 0.066(2) Uani 1 1 d .
H35A H 1.0794 0.6570 0.6524 0.079 Uiso 1 1 calc R
H35B H 1.1432 0.7350 0.6434 0.079 Uiso 1 1 calc R
C44 C 1.1134(6) 0.4732(8) 0.8255(5) 0.083(3) Uani 1 1 d .
H44A H 1.1331 0.4775 0.7910 0.100 Uiso 1 1 calc R
H44B H 1.1446 0.4263 0.8464 0.100 Uiso 1 1 calc R
C46 C 1.1784(6) 0.5700(7) 0.9399(5) 0.081(3) Uani 1 1 d .
H46A H 1.2150 0.5241 0.9276 0.097 Uiso 1 1 calc R
H46B H 1.1974 0.6339 0.9328 0.097 Uiso 1 1 calc R
C47 C 1.1769(8) 0.5593(8) 0.9933(4) 0.094(4) Uani 1 1 d .
H47A H 1.1395 0.6044 1.0054 0.112 Uiso 1 1 calc R
H47B H 1.2278 0.5761 1.0105 0.112 Uiso 1 1 calc R
O29 O 0.8112(4) 0.3249(4) 0.7109(2) 0.0635(17) Uani 1 1 d D
O30 O 1.0355(3) 0.3928(4) 0.9350(2) 0.0628(17) Uani 1 1 d .
C9 C 0.6467(4) 0.7813(5) 1.0433(3) 0.0460(17) Uani 1 1 d .
H9A H 0.6790 0.7296 1.0319 0.055 Uiso 1 1 calc R
H9B H 0.6479 0.7788 1.0816 0.055 Uiso 1 1 calc R
O27 O 0.7497(5) 0.1732(5) 0.7578(3) 0.094(2) Uani 1 1 d .
C24 C 0.3228(4) 0.3739(5) 0.4730(3) 0.0466(18) Uani 1 1 d .
H24A H 0.3571 0.4253 0.4637 0.056 Uiso 1 1 calc R
H24B H 0.2716 0.3849 0.4546 0.056 Uiso 1 1 calc R
C33 C 0.8165(5) 0.8035(7) 0.4661(3) 0.070(3) Uani 1 1 d .
H33A H 0.7771 0.7540 0.4672 0.084 Uiso 1 1 calc R
H33B H 0.8244 0.8156 0.4293 0.084 Uiso 1 1 calc R
C48 C 1.2105(5) 0.3948(7) 1.0085(4) 0.076(3) Uani 1 1 d .
H48A H 1.2592 0.4163 1.0272 0.091 Uiso 1 1 calc R
H48B H 1.2195 0.3823 0.9719 0.091 Uiso 1 1 calc R
C45 C 1.0249(7) 0.3590(8) 0.7912(4) 0.087(4) Uani 1 1 d .
H45A H 1.0682 0.3153 0.7996 0.105 Uiso 1 1 calc R
H45B H 1.0210 0.3722 0.7535 0.105 Uiso 1 1 calc R
C36 C 1.0472(6) 0.8154(6) 0.6945(3) 0.080(3) Uani 1 1 d .
H36A H 1.0896 0.8613 0.6996 0.096 Uiso 1 1 calc R
H36B H 1.0603 0.7601 0.7169 0.096 Uiso 1 1 calc R
H6 H 0.4293 0.4630 0.5862 0.040(18) Uiso 1 1 d R
H29D H 0.8158 0.3025 0.6751 0.08(3) Uiso 1 1 d R
H29C H 0.7806 0.2620 0.7248 0.11(4) Uiso 1 1 d RD
H1C H 0.7528 0.4225 0.7368 0.08(3) Uiso 1 1 d R
H2C H 0.7462 0.8011 0.7308 0.07(3) Uiso 1 1 d R
H2D H 0.7281 0.8032 0.7899 0.11(4) Uiso 1 1 d RD
H1D H 0.7358 0.4404 0.7916 0.05(2) Uiso 1 1 d RD
H28D H 0.5049 0.3477 0.5899 0.04(2) Uiso 1 1 d R
H30C H 1.0034 0.3611 0.9042 0.13(5) Uiso 1 1 d R
H28C H 0.4675 0.3356 0.5464 0.06(3) Uiso 1 1 d R
H30D H 1.0545 0.3392 0.9579 0.14(5) Uiso 1 1 d 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 N3 91.30(19) . .
O1 Ni1 O2 176.47(18) . .
N3 Ni1 O2 88.53(18) . .
O1 Ni1 N7 91.2(2) . .
N3 Ni1 N7 177.0(2) . .
O2 Ni1 N7 89.11(19) . .
O1 Ni1 N5 89.57(19) . .
N3 Ni1 N5 89.85(19) . .
O2 Ni1 N5 93.96(19) . .
N7 Ni1 N5 88.4(2) . .
O1 Ni1 N1 87.52(19) . .
N3 Ni1 N1 88.77(19) . .
O2 Ni1 N1 88.95(19) . .
N7 Ni1 N1 93.1(2) . .
N5 Ni1 N1 176.7(2) . .
O21 Cl3 O19 112.5(7) . .
O21 Cl3 O20 106.2(7) . .
O19 Cl3 O20 103.8(7) . .
O21 Cl3 O22 110.5(5) . .
O19 Cl3 O22 113.1(5) . .
O20 Cl3 O22 110.3(6) . .
O24 Cl4 O25 108.6(5) . .
O24 Cl4 O23 108.1(5) . .
O25 Cl4 O23 110.7(4) . .
O24 Cl4 O26 110.2(5) . .
O25 Cl4 O26 109.9(4) . .
O23 Cl4 O26 109.3(4) . .
O12 Cl1 O13 110.9(4) . .
O12 Cl1 O14 111.8(5) . .
O13 Cl1 O14 107.8(5) . .
O12 Cl1 O11 110.0(3) . .
O13 Cl1 O11 109.7(3) . .
O14 Cl1 O11 106.6(4) . .
O18 Cl2 O16 113.1(5) . .
O18 Cl2 O15 110.0(4) . .
O16 Cl2 O15 110.2(3) . .
O18 Cl2 O17 107.3(4) . .
O16 Cl2 O17 109.5(4) . .
O15 Cl2 O17 106.6(3) . .
Ni1 O2 H2C 129.2 . .
Ni1 O2 H2D 126.0 . .
H2C O2 H2D 104.6 . .
C25 N5 C29 118.1(5) . .
C25 N5 Ni1 120.4(4) . .
C29 N5 Ni1 121.5(4) . .
C18 N3 C14 117.5(5) . .
C18 N3 Ni1 121.8(4) . .
C14 N3 Ni1 120.6(4) . .
C41 N7 C37 117.5(5) . .
C41 N7 Ni1 122.5(4) . .
C37 N7 Ni1 119.8(4) . .
Ni1 O1 H1C 131.3 . .
Ni1 O1 H1D 113.5 . .
H1C O1 H1D 115.1 . .
C5 N1 C1 116.7(5) . .
C5 N1 Ni1 123.9(4) . .
C1 N1 Ni1 119.4(4) . .
C4 C3 C2 116.7(5) . .
C4 C3 C6 122.7(6) . .
C2 C3 C6 120.5(6) . .
C29 C28 C27 120.2(6) . .
C29 C28 H28 119.9 . .
C27 C28 H28 119.9 . .
N1 C5 C4 123.5(5) . .
N1 C5 H5 118.3 . .
C4 C5 H5 118.3 . .
C26 C27 C28 116.5(6) . .
C26 C27 C30 121.0(6) . .
C28 C27 C30 122.3(6) . .
C40 C39 C38 116.2(6) . .
C40 C39 C42 122.8(6) . .
C38 C39 C42 120.9(6) . .
N5 C29 C28 122.5(6) . .
N5 C29 H29 118.7 . .
C28 C29 H29 118.7 . .
C14 C15 C16 119.8(6) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
N3 C18 C17 122.9(5) . .
N3 C18 H18 118.6 . .
C17 C18 H18 118.6 . .
C3 C4 C5 119.2(6) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C1 C2 C3 120.3(6) . .
C1 C2 H2 119.9 . .
C3 C2 H2 119.9 . .
N3 C14 C15 123.1(6) . .
N3 C14 H14 118.5 . .
C15 C14 H14 118.5 . .
C37 C38 C39 121.0(6) . .
C37 C38 H38 119.5 . .
C39 C38 H38 119.5 . .
C41 C40 C39 119.9(6) . .
C41 C40 H40 120.0 . .
C39 C40 H40 120.0 . .
N1 C1 C2 123.7(6) . .
N1 C1 H1 118.2 . .
C2 C1 H1 118.2 . .
N7 C41 C40 123.2(6) . .
N7 C41 H41 118.4 . .
C40 C41 H41 118.4 . .
C27 C26 C25 120.8(6) . .
C27 C26 H26 119.6 . .
C25 C26 H26 119.6 . .
N5 C25 C26 121.8(6) . .
N5 C25 H25 119.1 . .
C26 C25 H25 119.1 . .
C18 C17 C16 119.7(6) . .
C18 C17 H17 120.1 . .
C16 C17 H17 120.1 . .
N7 C37 C38 122.2(6) . .
N7 C37 H37 118.9 . .
C38 C37 H37 118.9 . .
C19 N4 C20 112.6(5) . .
C19 N4 C22 107.1(5) . .
C20 N4 C22 111.8(5) . .
C19 N4 H6 107.1 . .
C20 N4 H6 111.5 . .
C22 N4 H6 106.5 . .
C34 N6 C30 112.6(6) . .
C34 N6 C31 112.8(6) . .
C30 N6 C31 110.7(6) . .
C10 N2 C6 112.8(5) . .
C10 N2 C7 108.2(5) . .
C6 N2 C7 111.4(5) . .
N2 C6 C3 114.5(5) . .
N2 C6 H6A 108.6 . .
C3 C6 H6A 108.6 . .
N2 C6 H6B 108.6 . .
C3 C6 H6B 108.6 . .
H6A C6 H6B 107.6 . .
C16 C19 N4 113.7(5) . .
C16 C19 H19A 108.8 . .
N4 C19 H19A 108.8 . .
C16 C19 H19B 108.8 . .
N4 C19 H19B 108.8 . .
H19A C19 H19B 107.7 . .
C15 C16 C17 117.0(6) . .
C15 C16 C19 120.5(6) . .
C17 C16 C19 122.4(5) . .
N6 C30 C27 113.6(5) . .
N6 C30 H30A 108.8 . .
C27 C30 H30A 108.8 . .
N6 C30 H30B 108.8 . .
C27 C30 H30B 108.8 . .
H30A C30 H30B 107.7 . .
C39 C42 N8 112.6(6) . .
C39 C42 H42A 109.1 . .
N8 C42 H42A 109.1 . .
C39 C42 H42B 109.1 . .
N8 C42 H42B 109.1 . .
H42A C42 H42B 107.8 . .
C46 N8 C42 114.8(7) . .
C46 N8 C43 105.6(8) . .
C42 N8 C43 111.6(6) . .
C46 N8 H8 108.2 . .
C42 N8 H8 108.2 . .
C43 N8 H8 108.2 . .
O4 C11 C10 107.9(5) . .
O4 C11 H11A 110.1 . .
C10 C11 H11A 110.1 . .
O4 C11 H11B 110.1 . .
C10 C11 H11B 110.1 . .
H11A C11 H11B 108.4 . .
N2 C10 C11 113.4(5) . .
N2 C10 H10A 108.9 . .
C11 C10 H10A 108.9 . .
N2 C10 H10B 108.9 . .
C11 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C44 C43 N8 112.7(8) . .
C44 C43 H43A 109.1 . .
N8 C43 H43A 109.1 . .
C44 C43 H43B 109.1 . .
N8 C43 H43B 109.1 . .
H43A C43 H43B 107.8 . .
C32 C31 N6 114.4(7) . .
C32 C31 H31A 108.7 . .
N6 C31 H31A 108.7 . .
C32 C31 H31B 108.7 . .
N6 C31 H31B 108.7 . .
H31A C31 H31B 107.6 . .
H28D O28 H28C 96.1 . .
C24 O6 C23 112.7(5) . .
C21 O5 C13 114.3(6) . 2_646
C12 O4 C11 113.1(5) . .
C8 O3 C9 113.1(5) . .
C44 O9 C45 113.8(8) . .
C36 O8 C35 111.8(7) . .
C23 C22 N4 113.5(5) . .
C23 C22 H22A 108.9 . .
N4 C22 H22A 108.9 . .
C23 C22 H22B 108.9 . .
N4 C22 H22B 108.9 . .
H22A C22 H22B 107.7 . .
C48 O10 C47 117.3(8) . .
C32 O7 C33 114.5(7) . .
O3 C8 C7 109.0(5) . .
O3 C8 H8A 109.9 . .
C7 C8 H8A 109.9 . .
O3 C8 H8B 109.9 . .
C7 C8 H8B 109.9 . .
H8A C8 H8B 108.3 . .
O5 C13 C12 111.5(6) 2_656 .
O5 C13 H13A 109.3 2_656 .
C12 C13 H13A 109.3 . .
O5 C13 H13B 109.3 2_656 .
C12 C13 H13B 109.3 . .
H13A C13 H13B 108.0 . .
N2 C7 C8 112.7(5) . .
N2 C7 H7A 109.0 . .
C8 C7 H7A 109.0 . .
N2 C7 H7B 109.0 . .
C8 C7 H7B 109.0 . .
H7A C7 H7B 107.8 . .
C21 C20 N4 112.6(5) . .
C21 C20 H20A 109.1 . .
N4 C20 H20A 109.1 . .
C21 C20 H20B 109.1 . .
N4 C20 H20B 109.1 . .
H20A C20 H20B 107.8 . .
O5 C21 C20 109.8(6) . .
O5 C21 H21A 109.7 . .
C20 C21 H21A 109.7 . .
O5 C21 H21B 109.7 . .
C20 C21 H21B 109.7 . .
H21A C21 H21B 108.2 . .
O6 C23 C22 114.8(5) . .
O6 C23 H23A 108.6 . .
C22 C23 H23A 108.6 . .
O6 C23 H23B 108.6 . .
C22 C23 H23B 108.6 . .
H23A C23 H23B 107.5 . .
O4 C12 C13 109.4(6) . .
O4 C12 H12A 109.8 . .
C13 C12 H12A 109.8 . .
O4 C12 H12B 109.8 . .
C13 C12 H12B 109.8 . .
H12A C12 H12B 108.2 . .
O7 C32 C31 110.9(7) . .
O7 C32 H32A 109.5 . .
C31 C32 H32A 109.5 . .
O7 C32 H32B 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 108.0 . .
N6 C34 C35 113.7(6) . .
N6 C34 H34A 108.8 . .
C35 C34 H34A 108.8 . .
N6 C34 H34B 108.8 . .
C35 C34 H34B 108.8 . .
H34A C34 H34B 107.7 . .
O8 C35 C34 107.1(6) . .
O8 C35 H35A 110.3 . .
C34 C35 H35A 110.3 . .
O8 C35 H35B 110.3 . .
C34 C35 H35B 110.3 . .
H35A C35 H35B 108.6 . .
O9 C44 C43 110.2(8) . .
O9 C44 H44A 109.6 . .
C43 C44 H44A 109.6 . .
O9 C44 H44B 109.6 . .
C43 C44 H44B 109.6 . .
H44A C44 H44B 108.1 . .
C47 C46 N8 114.1(10) . .
C47 C46 H46A 108.7 . .
N8 C46 H46A 108.7 . .
C47 C46 H46B 108.7 . .
N8 C46 H46B 108.7 . .
H46A C46 H46B 107.6 . .
C46 C47 O10 114.9(8) . .
C46 C47 H47A 108.6 . .
O10 C47 H47A 108.6 . .
C46 C47 H47B 108.6 . .
O10 C47 H47B 108.6 . .
H47A C47 H47B 107.5 . .
H29D O29 H29C 97.4 . .
H30C O30 H30D 104.6 . .
O3 C9 C24 109.6(6) . 2_656
O3 C9 H9A 109.8 . .
C24 C9 H9A 109.8 2_656 .
O3 C9 H9B 109.8 . .
C24 C9 H9B 109.8 2_656 .
H9A C9 H9B 108.2 . .
O6 C24 C9 109.2(6) . 2_646
O6 C24 H24A 109.8 . .
C9 C24 H24A 109.8 2_646 .
O6 C24 H24B 109.8 . .
C9 C24 H24B 109.8 2_646 .
H24A C24 H24B 108.3 . .
O7 C33 C48 109.4(7) . 2_756
O7 C33 H33A 109.8 . .
C48 C33 H33A 109.8 2_756 .
O7 C33 H33B 109.8 . .
C48 C33 H33B 109.8 2_756 .
H33A C33 H33B 108.2 . .
O10 C48 C33 109.7(8) . 2_746
O10 C48 H48A 109.7 . .
C33 C48 H48A 109.7 2_746 .
O10 C48 H48B 109.7 . .
C33 C48 H48B 109.7 2_746 .
H48A C48 H48B 108.2 . .
O9 C45 C36 108.5(7) . 2_746
O9 C45 H45A 110.0 . .
C36 C45 H45A 110.0 2_746 .
O9 C45 H45B 110.0 . .
C36 C45 H45B 110.0 2_746 .
H45A C45 H45B 108.4 . .
O8 C36 C45 108.6(8) . 2_756
O8 C36 H36A 110.0 . .
C45 C36 H36A 110.0 2_756 .
O8 C36 H36B 110.0 . .
C45 C36 H36B 110.0 2_756 .
H36A C36 H36B 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.096(4) .
Ni1 N3 2.097(5) .
Ni1 O2 2.106(4) .
Ni1 N7 2.109(5) .
Ni1 N5 2.112(5) .
Ni1 N1 2.113(5) .
Cl3 O21 1.383(7) .
Cl3 O19 1.385(8) .
Cl3 O20 1.397(8) .
Cl3 O22 1.410(7) .
Cl4 O24 1.413(7) .
Cl4 O25 1.417(6) .
Cl4 O23 1.424(6) .
Cl4 O26 1.425(6) .
Cl1 O12 1.402(6) .
Cl1 O13 1.415(6) .
Cl1 O14 1.441(7) .
Cl1 O11 1.455(5) .
Cl2 O18 1.414(6) .
Cl2 O16 1.413(6) .
Cl2 O15 1.452(5) .
Cl2 O17 1.459(6) .
O2 H2C 0.9207 .
O2 H2D 1.0858 .
N5 C25 1.326(8) .
N5 C29 1.344(8) .
N3 C18 1.349(8) .
N3 C14 1.349(7) .
N7 C41 1.339(8) .
N7 C37 1.347(8) .
O1 H1C 0.8576 .
O1 H1D 0.9169 .
N1 C5 1.338(8) .
N1 C1 1.338(8) .
C3 C4 1.391(9) .
C3 C2 1.394(9) .
C3 C6 1.511(8) .
C28 C29 1.380(8) .
C28 C27 1.384(9) .
C28 H28 0.9500 .
C5 C4 1.397(8) .
C5 H5 0.9500 .
C27 C26 1.379(9) .
C27 C30 1.516(9) .
C39 C40 1.394(9) .
C39 C38 1.393(9) .
C39 C42 1.492(10) .
C29 H29 0.9500 .
C15 C14 1.370(8) .
C15 C16 1.401(8) .
C15 H15 0.9500 .
C18 C17 1.373(9) .
C18 H18 0.9500 .
C4 H4 0.9500 .
C2 C1 1.371(9) .
C2 H2 0.9500 .
C14 H14 0.9500 .
C38 C37 1.373(9) .
C38 H38 0.9500 .
C40 C41 1.378(9) .
C40 H40 0.9500 .
C1 H1 0.9500 .
C41 H41 0.9500 .
C26 C25 1.395(9) .
C26 H26 0.9500 .
C25 H25 0.9500 .
C17 C16 1.403(9) .
C17 H17 0.9500 .
C37 H37 0.9500 .
N4 C19 1.509(8) .
N4 C20 1.517(8) .
N4 C22 1.517(8) .
N4 H6 1.0625 .
N6 C34 1.440(10) .
N6 C30 1.474(8) .
N6 C31 1.483(11) .
N2 C10 1.466(8) .
N2 C6 1.468(8) .
N2 C7 1.469(8) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C19 C16 1.502(9) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C42 N8 1.519(10) .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
N8 C46 1.477(11) .
N8 C43 1.598(13) .
N8 H8 0.9300 .
C11 O4 1.434(8) .
C11 C10 1.518(10) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C43 C44 1.408(14) .
C43 H43A 0.9900 .
C43 H43B 0.9900 .
C31 C32 1.468(14) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
O28 H28D 0.8248 .
O28 H28C 0.8684 .
O6 C24 1.406(8) .
O6 C23 1.416(8) .
O5 C21 1.400(8) .
O5 C13 1.419(8) 2_646
O4 C12 1.413(8) .
O3 C8 1.421(8) .
O3 C9 1.426(8) .
O9 C44 1.393(12) .
O9 C45 1.427(12) .
O8 C36 1.346(10) .
O8 C35 1.446(10) .
C22 C23 1.508(9) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
O10 C48 1.354(11) .
O10 C47 1.495(12) .
O7 C32 1.405(10) .
O7 C33 1.410(10) .
C8 C7 1.512(10) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C13 O5 1.419(8) 2_656
C13 C12 1.462(11) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C20 C21 1.479(10) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C34 C35 1.513(13) .
C34 H34A 0.9900 .
C34 H34B 0.9900 .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C44 H44A 0.9900 .
C44 H44B 0.9900 .
C46 C47 1.393(15) .
C46 H46A 0.9900 .
C46 H46B 0.9900 .
C47 H47A 0.9900 .
C47 H47B 0.9900 .
O29 H29D 0.9900 .
O29 H29C 1.1192 .
O30 H30C 1.0350 .
O30 H30D 1.0014 .
C9 C24 1.495(10) 2_656
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C24 C9 1.495(10) 2_646
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C33 C48 1.549(14) 2_756
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C48 C33 1.549(14) 2_746
C48 H48A 0.9900 .
C48 H48B 0.9900 .
C45 C36 1.488(15) 2_746
C45 H45A 0.9900 .
C45 H45B 0.9900 .
C36 C45 1.488(15) 2_756
C36 H36A 0.9900 .
C36 H36B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8 O30 0.93 1.81 2.723(8) 167.7 .
N4 H6 O28 1.06 1.67 2.702(7) 162.4 .
O1 H1D O20 0.92 2.22 2.939(12) 134.3 .
O1 H1C O29 0.86 1.89 2.660(7) 149.3 .
O29 H29C O27 1.12 1.64 2.745(9) 166.2 .
O2 H2D O11 1.09 1.93 2.792(6) 133.9 .
O2 H2C O15 0.92 1.86 2.739(7) 158.0 .
O28 H28C O3 0.87 2.02 2.840(6) 156.1 2_646
O28 H28D O4 0.82 1.98 2.797(6) 171.6 2_646
O30 H30D O7 1.00 1.83 2.791(7) 159.7 2_746
O30 H30C O8 1.04 1.73 2.747(7) 167.9 2_746
