#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:11:05 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261652 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/63/7706325.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_7706325
loop_
_publ_author_name
'Deorukhkar, Neel'
'Besnard, Céline'
'Guénée, Laure'
'Piguet, Claude'
_publ_section_title
;
 Tuning spin-crossover transition temperatures in non-symmetrical
 homoleptic meridional/facial [Fe(didentate)₃]²⁺
 complexes: what for and who cares about it?
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1206
_journal_page_last               1223
_journal_paper_doi               10.1039/d0dt03828h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C36 H30 N12 Ni, 2(Cl O4), C2 H3 N'
_chemical_formula_sum            'C38 H33 Cl2 N13 Ni O8'
_chemical_formula_weight         929.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-05 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.51580(10)
_cell_length_b                   22.5839(2)
_cell_length_c                   19.1174(2)
_cell_measurement_reflns_used    20416
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      68.9230
_cell_measurement_theta_min      2.2720
_cell_volume                     4081.33(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00  -2.00   1.00    1.00    --  -38.13 125.00   0.00   84
  2  ω    -10.00  41.00   1.00    1.00    --  -38.13  38.00 120.00   51
  3  ω   -123.00 -80.00   1.00    1.00    --  -38.13 -84.00  48.00   43
  4  ω     11.00 105.00   1.00    1.00    --   38.13  57.00-120.00   94
  5  ω     32.00  58.00   1.00    1.00    --   38.13-125.00-180.00   26
  6  ω      1.00  49.00   1.00    1.00    --   38.13 -99.00 -30.00   48
  7  ω      3.00  71.00   1.00    1.00    --   38.13 -99.00-120.00   68
  8  ω     79.00 108.00   1.00    4.00    --  100.00-111.00 -60.00   29
  9  ω     81.00 151.00   1.00    4.00    --  100.00 178.00 120.00   70
 10  ω     24.00 112.00   1.00    4.00    --  100.00 -61.00 150.00   88
 11  ω     42.00 117.00   1.00    4.00    --  100.00 -77.00  90.00   75
 12  ω     85.00 112.00   1.00    4.00    --  100.00-111.00  90.00   27
 13  ω     21.00 121.00   1.00    4.00    --  100.00 -30.00 150.00  100
 14  ω     67.00 118.00   1.00    4.00    --  100.00  77.00 -90.00   51
 15  ω    101.00 178.00   1.00    4.00    --  100.00 111.00-180.00   77
 16  ω     88.00 113.00   1.00    4.00    --  100.00-111.00-180.00   25
 17  ω     91.00 178.00   1.00    4.00    --  100.00  77.00-120.00   87
 18  ω     58.00  83.00   1.00    4.00    --  100.00 178.00   0.00   25
 19  ω     99.00 142.00   1.00    4.00    --  100.00 178.00   0.00   43
 20  ω     88.00 113.00   1.00    4.00    --  100.00-111.00  30.00   25
 21  ω    100.00 144.00   1.00    4.00    --  100.00 111.00  60.00   44
 22  ω     37.00  64.00   1.00    4.00    --  100.00-111.00-180.00   27
 23  ω     97.00 149.00   1.00    4.00    --  100.00  45.00-120.00   52
 24  ω    144.00 169.00   1.00    4.00    --  100.00  77.00 -90.00   25
 25  ω     24.00  58.00   1.00    4.00    --  100.00 -94.00  90.00   34
 26  ω     12.00 175.00   1.00    4.00    --  100.00   0.00  60.00  163
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1544003000
_diffrn_orient_matrix_UB_12      -0.0191123000
_diffrn_orient_matrix_UB_13      0.0212247000
_diffrn_orient_matrix_UB_21      0.0263445000
_diffrn_orient_matrix_UB_22      0.0570868000
_diffrn_orient_matrix_UB_23      0.0437239000
_diffrn_orient_matrix_UB_31      -0.0449415000
_diffrn_orient_matrix_UB_32      -0.0320821000
_diffrn_orient_matrix_UB_33      0.0649507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0140
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.897
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0468
_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)+(0.0715P)²+3.9109P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7166
_reflns_number_total             7537
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt03828h2.cif
_cod_data_source_block           4_NiL6ClO4
_cod_depositor_comments
'Adding full bibliography for 7706322--7706338.cif.'
_cod_database_code               7706325
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H33 Cl2 N13 Ni O8'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2A-O5A \\sim Cl2B-O5B
 with sigma of 0.02
 Cl2B-O7B \\sim Cl2A-O7A
 with sigma of 0.02
 Cl2A-O8A \\sim Cl2B-O8B
 with sigma of 0.02
 Cl2B-O6B \\sim Cl2A-O6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl2B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
4. Rigid body (RIGU) restrains
 Cl2A, O6A, O5A, O8A, O7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2B, O8B, O7B, O5B, O6B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cl2B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(O8B)=1-FVAR(1)
 Sof(Cl2A)=Sof(O8A)=Sof(O7A)=Sof(O5A)=Sof(O6A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C34(H34), C35(H35), C36(H36)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.876
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.41105(4) 0.31654(2) 0.68339(2) 0.02847(12) Uani 1 1 d . . . . .
N1 N 0.5147(2) 0.37064(8) 0.61915(10) 0.0313(4) Uani 1 1 d . . . . .
N2 N 0.5549(2) 0.39548(9) 0.51014(10) 0.0325(4) Uani 1 1 d . . . . .
N3 N 0.3455(2) 0.27993(8) 0.58157(10) 0.0327(4) Uani 1 1 d . . . . .
N4 N 0.3965(2) 0.28585(9) 0.46318(10) 0.0371(4) Uani 1 1 d . . . . .
N5 N 0.5570(2) 0.24854(8) 0.69766(10) 0.0320(4) Uani 1 1 d . . . . .
N6 N 0.6038(2) 0.15577(8) 0.73249(10) 0.0360(4) Uani 1 1 d . . . . .
N7 N 0.2985(2) 0.25320(8) 0.73434(10) 0.0316(4) Uani 1 1 d . . . . .
N8 N 0.3262(3) 0.16075(9) 0.79381(11) 0.0424(5) Uani 1 1 d . . . . .
N9 N 0.45949(19) 0.35876(8) 0.77966(10) 0.0304(4) Uani 1 1 d . . . . .
N10 N 0.3932(2) 0.42434(9) 0.85721(10) 0.0339(4) Uani 1 1 d . . . . .
N11 N 0.2531(2) 0.38308(8) 0.67881(10) 0.0314(4) Uani 1 1 d . . . . .
N12 N 0.1994(2) 0.47303(9) 0.73538(12) 0.0406(5) Uani 1 1 d . . . . .
C1 C 0.5953(2) 0.42149(10) 0.62305(12) 0.0317(5) Uani 1 1 d . . . . .
C2 C 0.6485(3) 0.45586(11) 0.68111(13) 0.0365(5) Uani 1 1 d . . . . .
H2 H 0.632500 0.445415 0.727677 0.044 Uiso 1 1 calc R U . . .
C3 C 0.7252(3) 0.50556(12) 0.66757(14) 0.0417(6) Uani 1 1 d . . . . .
H3 H 0.761262 0.530289 0.705660 0.050 Uiso 1 1 calc R U . . .
C4 C 0.7514(3) 0.52059(11) 0.59884(15) 0.0435(6) Uani 1 1 d . . . . .
H4 H 0.805794 0.554933 0.591884 0.052 Uiso 1 1 calc R U . . .
C5 C 0.7008(3) 0.48707(11) 0.54153(14) 0.0400(5) Uani 1 1 d . . . . .
H5 H 0.718975 0.497255 0.495207 0.048 Uiso 1 1 calc R U . . .
C6 C 0.6214(2) 0.43747(10) 0.55477(12) 0.0303(4) Uani 1 1 d . . . . .
C7 C 0.4920(2) 0.35652(10) 0.55125(11) 0.0289(4) Uani 1 1 d . . . . .
C8 C 0.5576(3) 0.39461(13) 0.43385(12) 0.0422(6) Uani 1 1 d . . . . .
H8A H 0.624935 0.364521 0.421671 0.063 Uiso 1 1 calc R U . . .
H8B H 0.586744 0.433545 0.418054 0.063 Uiso 1 1 calc R U . . .
H8C H 0.463031 0.385174 0.410687 0.063 Uiso 1 1 calc R U . . .
C9 C 0.4065(2) 0.30480(10) 0.52904(12) 0.0312(5) Uani 1 1 d . . . . .
C10 C 0.3193(3) 0.23697(11) 0.44867(14) 0.0426(6) Uani 1 1 d . . . . .
H10 H 0.309242 0.222059 0.401897 0.051 Uiso 1 1 calc R U . . .
C11 C 0.2536(3) 0.20730(12) 0.49935(14) 0.0453(6) Uani 1 1 d . . . . .
H11 H 0.199886 0.172377 0.488443 0.054 Uiso 1 1 calc R U . . .
C12 C 0.2697(3) 0.23070(11) 0.56617(13) 0.0384(5) Uani 1 1 d . . . . .
H12 H 0.226033 0.211518 0.602265 0.046 Uiso 1 1 calc R U . . .
C13 C 0.6849(2) 0.23237(10) 0.67541(12) 0.0330(5) Uani 1 1 d . . . . .
C14 C 0.7763(2) 0.26294(12) 0.63610(13) 0.0386(5) Uani 1 1 d . . . . .
H14 H 0.758858 0.302907 0.622223 0.046 Uiso 1 1 calc R U . . .
C15 C 0.8928(3) 0.23270(13) 0.61823(15) 0.0447(6) Uani 1 1 d . . . . .
H15 H 0.956111 0.252099 0.590766 0.054 Uiso 1 1 calc R U . . .
C16 C 0.9206(3) 0.17354(13) 0.63977(15) 0.0467(6) Uani 1 1 d . . . . .
H16 H 1.001859 0.154126 0.626269 0.056 Uiso 1 1 calc R U . . .
C17 C 0.8330(3) 0.14344(12) 0.67973(14) 0.0434(6) Uani 1 1 d . . . . .
H17 H 0.852518 0.103930 0.694901 0.052 Uiso 1 1 calc R U . . .
C18 C 0.7142(3) 0.17371(11) 0.69690(12) 0.0354(5) Uani 1 1 d . . . . .
C19 C 0.5114(3) 0.20163(10) 0.73029(11) 0.0324(5) Uani 1 1 d . . . . .
C20 C 0.5911(4) 0.09560(11) 0.75997(14) 0.0487(7) Uani 1 1 d . . . . .
H20A H 0.667603 0.088402 0.797846 0.073 Uiso 1 1 calc R U . . .
H20B H 0.597447 0.066881 0.722026 0.073 Uiso 1 1 calc R U . . .
H20C H 0.499639 0.091305 0.778382 0.073 Uiso 1 1 calc R U . . .
C21 C 0.3717(3) 0.20402(10) 0.75542(11) 0.0326(5) Uani 1 1 d . . . . .
C22 C 0.1955(3) 0.16723(12) 0.81179(15) 0.0479(6) Uani 1 1 d . . . . .
H22 H 0.158886 0.137058 0.839216 0.057 Uiso 1 1 calc R U . . .
C23 C 0.1112(3) 0.21542(12) 0.79262(13) 0.0429(6) Uani 1 1 d . . . . .
H23 H 0.018247 0.218690 0.805753 0.052 Uiso 1 1 calc R U . . .
C24 C 0.1679(3) 0.25863(11) 0.75353(12) 0.0352(5) Uani 1 1 d . . . . .
H24 H 0.113576 0.292887 0.739914 0.042 Uiso 1 1 calc R U . . .
C25 C 0.5381(2) 0.34847(10) 0.84424(12) 0.0336(5) Uani 1 1 d . . . . .
C26 C 0.6401(3) 0.30532(12) 0.86521(14) 0.0426(6) Uani 1 1 d . . . . .
H26 H 0.671994 0.278156 0.832534 0.051 Uiso 1 1 calc R U . . .
C27 C 0.6920(3) 0.30417(14) 0.93585(16) 0.0556(7) Uani 1 1 d . . . . .
H27 H 0.760590 0.275264 0.952114 0.067 Uiso 1 1 calc R U . . .
C28 C 0.6458(3) 0.34474(15) 0.98416(16) 0.0569(8) Uani 1 1 d . . . . .
H28 H 0.682602 0.341788 1.032365 0.068 Uiso 1 1 calc R U . . .
C29 C 0.5493(3) 0.38839(13) 0.96405(14) 0.0478(6) Uani 1 1 d . . . . .
H29 H 0.520590 0.416448 0.996602 0.057 Uiso 1 1 calc R U . . .
C30 C 0.4960(3) 0.38918(11) 0.89307(13) 0.0362(5) Uani 1 1 d . . . . .
C31 C 0.3746(2) 0.40365(9) 0.79029(12) 0.0299(4) Uani 1 1 d . . . . .
C32 C 0.3226(3) 0.47326(12) 0.88972(14) 0.0436(6) Uani 1 1 d . . . . .
H32A H 0.386149 0.507519 0.895212 0.065 Uiso 1 1 calc R U . . .
H32B H 0.298589 0.460887 0.936022 0.065 Uiso 1 1 calc R U . . .
H32C H 0.236039 0.484052 0.859639 0.065 Uiso 1 1 calc R U . . .
C33 C 0.2686(2) 0.42219(10) 0.73259(12) 0.0311(5) Uani 1 1 d . . . . .
C34 C 0.1048(3) 0.48496(12) 0.67988(16) 0.0503(7) Uani 1 1 d . . . . .
H34 H 0.052732 0.520852 0.679830 0.060 Uiso 1 1 calc R U . . .
C35 C 0.0795(3) 0.44786(13) 0.62303(16) 0.0516(7) Uani 1 1 d . . . . .
H35 H 0.011341 0.457274 0.584350 0.062 Uiso 1 1 calc R U . . .
C36 C 0.1575(3) 0.39618(12) 0.62453(13) 0.0398(5) Uani 1 1 d . . . . .
H36 H 0.142590 0.369412 0.586060 0.048 Uiso 1 1 calc R U . . .
Cl1 Cl 0.05917(7) 0.64203(3) 0.55015(3) 0.04608(17) Uani 1 1 d . . . . .
O1 O -0.0850(2) 0.65832(14) 0.53657(12) 0.0785(8) Uani 1 1 d . . . . .
O2 O 0.1248(3) 0.6655(2) 0.61280(17) 0.1298(17) Uani 1 1 d . . . . .
O3 O 0.1343(3) 0.65378(14) 0.49297(13) 0.0778(8) Uani 1 1 d . . . . .
O4 O 0.0656(4) 0.58032(15) 0.5579(3) 0.1345(17) Uani 1 1 d . . . . .
Cl2A Cl 0.2915(4) 0.06442(13) 0.61814(11) 0.0470(7) Uani 0.602(11) 1 d D U P A
1
O8A O 0.2048(9) 0.0917(4) 0.6602(3) 0.115(3) Uani 0.602(11) 1 d D . P A 1
O7A O 0.4131(9) 0.1053(3) 0.6168(4) 0.087(2) Uani 0.602(11) 1 d D . P A 1
O5A O 0.3467(6) 0.0121(2) 0.6541(3) 0.0711(15) Uani 0.602(11) 1 d D . P A 1
O6A O 0.2340(10) 0.0534(4) 0.5499(3) 0.096(3) Uani 0.602(11) 1 d D . P A 1
Cl2B Cl 0.2621(10) 0.0629(3) 0.6156(4) 0.101(3) Uani 0.398(11) 1 d D U P A 2
O5B O 0.3536(8) 0.0183(4) 0.6045(10) 0.115(4) Uani 0.398(11) 1 d D . P A 2
O6B O 0.1742(11) 0.0722(6) 0.5510(5) 0.083(3) Uani 0.398(11) 1 d D . P A 2
O7B O 0.3384(13) 0.1170(3) 0.6316(5) 0.078(3) Uani 0.398(11) 1 d D . P A 2
O8B O 0.1634(12) 0.0537(6) 0.6648(5) 0.104(3) Uani 0.398(11) 1 d D . P A 2
N13 N 0.0705(5) 0.36330(18) 0.8439(2) 0.1044(14) Uani 1 1 d . . . . .
C37 C 0.0045(4) 0.39217(16) 0.8738(2) 0.0722(10) Uani 1 1 d . . . . .
C38 C -0.0700(5) 0.4286(2) 0.9178(4) 0.122(2) Uani 1 1 d . . . . .
H38A H -0.057295 0.470279 0.905731 0.182 Uiso 1 1 calc R U . . .
H38B H -0.033202 0.421936 0.967140 0.182 Uiso 1 1 calc R U . . .
H38C H -0.170902 0.418651 0.910743 0.182 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0902
1 0 0 0.0902
0 3 -5 0.1100
0 -1 0 0.0878
0 1 0 0.1299
0 1 1 0.0997
0 0 -1 0.0982
0 -1 3 0.1044
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 Ni1 N3 78.27(7) . . ?
N1 Ni1 N5 99.14(8) . . ?
N1 Ni1 N7 170.87(8) . . ?
N1 Ni1 N9 100.54(7) . . ?
N1 Ni1 N11 86.60(7) . . ?
N5 Ni1 N3 87.38(7) . . ?
N5 Ni1 N7 78.62(8) . . ?
N5 Ni1 N9 98.43(7) . . ?
N5 Ni1 N11 173.84(8) . . ?
N7 Ni1 N3 92.75(7) . . ?
N7 Ni1 N11 96.06(7) . . ?
N9 Ni1 N3 174.19(7) . . ?
N9 Ni1 N7 88.56(7) . . ?
N9 Ni1 N11 78.20(7) . . ?
N11 Ni1 N3 96.03(7) . . ?
C1 N1 Ni1 139.71(16) . . ?
C7 N1 Ni1 113.83(15) . . ?
C7 N1 C1 106.24(19) . . ?
C6 N2 C8 124.5(2) . . ?
C7 N2 C6 106.73(18) . . ?
C7 N2 C8 128.7(2) . . ?
C9 N3 Ni1 114.45(15) . . ?
C9 N3 C12 116.8(2) . . ?
C12 N3 Ni1 127.87(16) . . ?
C9 N4 C10 116.3(2) . . ?
C13 N5 Ni1 139.17(16) . . ?
C19 N5 Ni1 113.87(15) . . ?
C19 N5 C13 106.24(19) . . ?
C18 N6 C20 123.3(2) . . ?
C19 N6 C18 106.77(19) . . ?
C19 N6 C20 129.7(2) . . ?
C21 N7 Ni1 115.33(15) . . ?
C24 N7 Ni1 127.18(16) . . ?
C24 N7 C21 117.2(2) . . ?
C21 N8 C22 115.8(2) . . ?
C25 N9 Ni1 138.91(16) . . ?
C31 N9 Ni1 114.17(15) . . ?
C31 N9 C25 105.49(19) . . ?
C30 N10 C32 123.8(2) . . ?
C31 N10 C30 106.19(19) . . ?
C31 N10 C32 130.1(2) . . ?
C33 N11 Ni1 114.65(15) . . ?
C36 N11 Ni1 127.38(17) . . ?
C36 N11 C33 116.9(2) . . ?
C33 N12 C34 115.7(2) . . ?
N1 C1 C2 130.8(2) . . ?
N1 C1 C6 108.7(2) . . ?
C2 C1 C6 120.5(2) . . ?
C1 C2 H2 121.5 . . ?
C3 C2 C1 117.0(2) . . ?
C3 C2 H2 121.5 . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.7(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 119.0 . . ?
C5 C4 C3 121.9(2) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 121.7 . . ?
C4 C5 C6 116.6(2) . . ?
C6 C5 H5 121.7 . . ?
N2 C6 C1 106.31(19) . . ?
N2 C6 C5 131.4(2) . . ?
C5 C6 C1 122.3(2) . . ?
N1 C7 N2 112.0(2) . . ?
N1 C7 C9 119.9(2) . . ?
N2 C7 C9 128.1(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C7 113.12(19) . . ?
N4 C9 N3 126.0(2) . . ?
N4 C9 C7 120.8(2) . . ?
N4 C10 H10 118.8 . . ?
N4 C10 C11 122.4(2) . . ?
C11 C10 H10 118.8 . . ?
C10 C11 H11 121.5 . . ?
C12 C11 C10 116.9(2) . . ?
C12 C11 H11 121.5 . . ?
N3 C12 C11 121.6(2) . . ?
N3 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
N5 C13 C14 131.3(2) . . ?
N5 C13 C18 108.1(2) . . ?
C14 C13 C18 120.6(2) . . ?
C13 C14 H14 121.4 . . ?
C15 C14 C13 117.2(2) . . ?
C15 C14 H14 121.4 . . ?
C14 C15 H15 119.2 . . ?
C14 C15 C16 121.6(3) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 H16 119.2 . . ?
C17 C16 C15 121.6(2) . . ?
C17 C16 H16 119.2 . . ?
C16 C17 H17 121.7 . . ?
C16 C17 C18 116.7(2) . . ?
C18 C17 H17 121.7 . . ?
N6 C18 C13 106.6(2) . . ?
N6 C18 C17 131.2(2) . . ?
C17 C18 C13 122.2(2) . . ?
N5 C19 N6 112.3(2) . . ?
N5 C19 C21 118.8(2) . . ?
N6 C19 C21 128.8(2) . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N7 C21 C19 112.91(19) . . ?
N8 C21 N7 125.7(2) . . ?
N8 C21 C19 121.4(2) . . ?
N8 C22 H22 118.3 . . ?
N8 C22 C23 123.3(2) . . ?
C23 C22 H22 118.3 . . ?
C22 C23 H23 121.5 . . ?
C24 C23 C22 116.9(2) . . ?
C24 C23 H23 121.5 . . ?
N7 C24 C23 121.1(2) . . ?
N7 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
N9 C25 C26 131.0(2) . . ?
N9 C25 C30 108.5(2) . . ?
C30 C25 C26 120.5(2) . . ?
C25 C26 H26 121.6 . . ?
C27 C26 C25 116.8(3) . . ?
C27 C26 H26 121.6 . . ?
C26 C27 H27 119.2 . . ?
C26 C27 C28 121.7(3) . . ?
C28 C27 H27 119.2 . . ?
C27 C28 H28 118.9 . . ?
C29 C28 C27 122.3(3) . . ?
C29 C28 H28 118.9 . . ?
C28 C29 H29 122.0 . . ?
C28 C29 C30 116.1(3) . . ?
C30 C29 H29 122.0 . . ?
N10 C30 C25 106.7(2) . . ?
N10 C30 C29 130.5(2) . . ?
C29 C30 C25 122.7(2) . . ?
N9 C31 N10 113.1(2) . . ?
N9 C31 C33 118.7(2) . . ?
N10 C31 C33 128.0(2) . . ?
N10 C32 H32A 109.5 . . ?
N10 C32 H32B 109.5 . . ?
N10 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N11 C33 C31 113.03(19) . . ?
N12 C33 N11 125.8(2) . . ?
N12 C33 C31 121.2(2) . . ?
N12 C34 H34 118.4 . . ?
N12 C34 C35 123.1(2) . . ?
C35 C34 H34 118.4 . . ?
C34 C35 H35 121.5 . . ?
C34 C35 C36 117.0(2) . . ?
C36 C35 H35 121.5 . . ?
N11 C36 C35 121.4(2) . . ?
N11 C36 H36 119.3 . . ?
C35 C36 H36 119.3 . . ?
O2 Cl1 O1 112.91(17) . . ?
O2 Cl1 O3 112.4(2) . . ?
O2 Cl1 O4 106.1(3) . . ?
O3 Cl1 O1 112.28(15) . . ?
O3 Cl1 O4 104.6(2) . . ?
O4 Cl1 O1 107.9(2) . . ?
O8A Cl2A O7A 104.8(5) . . ?
O8A Cl2A O5A 107.6(4) . . ?
O8A Cl2A O6A 116.0(6) . . ?
O5A Cl2A O7A 106.1(4) . . ?
O6A Cl2A O7A 108.8(5) . . ?
O6A Cl2A O5A 112.8(5) . . ?
O5B Cl2B O6B 107.2(9) . . ?
O5B Cl2B O7B 110.2(7) . . ?
O5B Cl2B O8B 118.5(9) . . ?
O6B Cl2B O7B 106.9(9) . . ?
O8B Cl2B O6B 103.2(9) . . ?
O8B Cl2B O7B 110.0(8) . . ?
N13 C37 C38 174.4(6) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
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
Ni1 N1 2.0620(19) . ?
Ni1 N3 2.1408(19) . ?
Ni1 N5 2.0672(19) . ?
Ni1 N7 2.0931(19) . ?
Ni1 N9 2.0771(19) . ?
Ni1 N11 2.1199(19) . ?
N1 C1 1.378(3) . ?
N1 C7 1.330(3) . ?
N2 C6 1.380(3) . ?
N2 C7 1.363(3) . ?
N2 C8 1.462(3) . ?
N3 C9 1.339(3) . ?
N3 C12 1.340(3) . ?
N4 C9 1.323(3) . ?
N4 C10 1.337(3) . ?
N5 C13 1.384(3) . ?
N5 C19 1.327(3) . ?
N6 C18 1.376(3) . ?
N6 C19 1.356(3) . ?
N6 C20 1.467(3) . ?
N7 C21 1.348(3) . ?
N7 C24 1.341(3) . ?
N8 C21 1.324(3) . ?
N8 C22 1.336(4) . ?
N9 C25 1.388(3) . ?
N9 C31 1.326(3) . ?
N10 C30 1.380(3) . ?
N10 C31 1.354(3) . ?
N10 C32 1.467(3) . ?
N11 C33 1.351(3) . ?
N11 C36 1.333(3) . ?
N12 C33 1.328(3) . ?
N12 C34 1.338(3) . ?
C1 C2 1.401(3) . ?
C1 C6 1.404(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.407(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.373(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(3) . ?
C7 C9 1.459(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.385(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.375(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(4) . ?
C13 C18 1.406(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.414(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.373(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(3) . ?
C19 C21 1.466(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 H22 0.9500 . ?
C22 C23 1.376(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.376(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.401(3) . ?
C25 C30 1.401(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.407(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.372(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.393(4) . ?
C31 C33 1.468(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C34 H34 0.9500 . ?
C34 C35 1.372(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(4) . ?
C36 H36 0.9500 . ?
Cl1 O1 1.415(2) . ?
Cl1 O2 1.391(3) . ?
Cl1 O3 1.399(2) . ?
Cl1 O4 1.402(3) . ?
Cl2A O8A 1.364(6) . ?
Cl2A O7A 1.482(6) . ?
Cl2A O5A 1.436(5) . ?
Cl2A O6A 1.378(5) . ?
Cl2B O5B 1.364(9) . ?
Cl2B O6B 1.426(10) . ?
Cl2B O7B 1.435(9) . ?
Cl2B O8B 1.418(10) . ?
N13 C37 1.108(5) . ?
C37 C38 1.422(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C1 C2 5.6(4) . . . . ?
Ni1 N1 C1 C6 -174.19(17) . . . . ?
Ni1 N1 C7 N2 176.10(14) . . . . ?
Ni1 N1 C7 C9 -3.1(3) . . . . ?
Ni1 N3 C9 N4 171.70(18) . . . . ?
Ni1 N3 C9 C7 -7.0(2) . . . . ?
Ni1 N3 C12 C11 -169.76(19) . . . . ?
Ni1 N5 C13 C14 7.8(4) . . . . ?
Ni1 N5 C13 C18 -169.62(18) . . . . ?
Ni1 N5 C19 N6 173.80(15) . . . . ?
Ni1 N5 C19 C21 -3.3(3) . . . . ?
Ni1 N7 C21 N8 173.76(19) . . . . ?
Ni1 N7 C21 C19 -7.3(2) . . . . ?
Ni1 N7 C24 C23 -173.91(18) . . . . ?
Ni1 N9 C25 C26 12.6(4) . . . . ?
Ni1 N9 C25 C30 -164.76(18) . . . . ?
Ni1 N9 C31 N10 169.96(14) . . . . ?
Ni1 N9 C31 C33 -6.0(3) . . . . ?
Ni1 N11 C33 N12 167.56(19) . . . . ?
Ni1 N11 C33 C31 -11.6(2) . . . . ?
Ni1 N11 C36 C35 -166.6(2) . . . . ?
N1 C1 C2 C3 -179.1(2) . . . . ?
N1 C1 C6 N2 0.2(2) . . . . ?
N1 C1 C6 C5 -179.8(2) . . . . ?
N1 C7 C9 N3 6.9(3) . . . . ?
N1 C7 C9 N4 -171.8(2) . . . . ?
N2 C7 C9 N3 -172.2(2) . . . . ?
N2 C7 C9 N4 9.1(3) . . . . ?
N4 C10 C11 C12 0.7(4) . . . . ?
N5 C13 C14 C15 -175.6(2) . . . . ?
N5 C13 C18 N6 -0.6(2) . . . . ?
N5 C13 C18 C17 177.1(2) . . . . ?
N5 C19 C21 N7 7.1(3) . . . . ?
N5 C19 C21 N8 -173.8(2) . . . . ?
N6 C19 C21 N7 -169.5(2) . . . . ?
N6 C19 C21 N8 9.6(4) . . . . ?
N8 C22 C23 C24 -0.7(4) . . . . ?
N9 C25 C26 C27 -175.1(3) . . . . ?
N9 C25 C30 N10 -0.7(3) . . . . ?
N9 C25 C30 C29 176.3(2) . . . . ?
N9 C31 C33 N11 11.9(3) . . . . ?
N9 C31 C33 N12 -167.3(2) . . . . ?
N10 C31 C33 N11 -163.3(2) . . . . ?
N10 C31 C33 N12 17.4(4) . . . . ?
N12 C34 C35 C36 -0.3(5) . . . . ?
C1 N1 C7 N2 0.5(2) . . . . ?
C1 N1 C7 C9 -178.75(19) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C2 C1 C6 N2 -179.6(2) . . . . ?
C2 C1 C6 C5 0.4(3) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C4 C5 C6 N2 179.2(2) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C6 N2 C7 N1 -0.4(2) . . . . ?
C6 N2 C7 C9 178.8(2) . . . . ?
C6 C1 C2 C3 0.6(3) . . . . ?
C7 N1 C1 C2 179.3(2) . . . . ?
C7 N1 C1 C6 -0.4(2) . . . . ?
C7 N2 C6 C1 0.1(2) . . . . ?
C7 N2 C6 C5 -179.9(2) . . . . ?
C8 N2 C6 C1 -178.7(2) . . . . ?
C8 N2 C6 C5 1.2(4) . . . . ?
C8 N2 C7 N1 178.4(2) . . . . ?
C8 N2 C7 C9 -2.4(4) . . . . ?
C9 N3 C12 C11 -0.9(3) . . . . ?
C9 N4 C10 C11 -0.3(4) . . . . ?
C10 N4 C9 N3 -0.7(3) . . . . ?
C10 N4 C9 C7 177.9(2) . . . . ?
C10 C11 C12 N3 0.0(4) . . . . ?
C12 N3 C9 N4 1.3(3) . . . . ?
C12 N3 C9 C7 -177.36(19) . . . . ?
C13 N5 C19 N6 1.6(3) . . . . ?
C13 N5 C19 C21 -175.57(19) . . . . ?
C13 C14 C15 C16 -1.1(4) . . . . ?
C14 C13 C18 N6 -178.4(2) . . . . ?
C14 C13 C18 C17 -0.7(4) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C16 C17 C18 N6 176.4(2) . . . . ?
C16 C17 C18 C13 -0.7(4) . . . . ?
C18 N6 C19 N5 -2.0(3) . . . . ?
C18 N6 C19 C21 174.8(2) . . . . ?
C18 C13 C14 C15 1.5(3) . . . . ?
C19 N5 C13 C14 176.9(2) . . . . ?
C19 N5 C13 C18 -0.5(2) . . . . ?
C19 N6 C18 C13 1.5(2) . . . . ?
C19 N6 C18 C17 -175.9(2) . . . . ?
C20 N6 C18 C13 176.4(2) . . . . ?
C20 N6 C18 C17 -1.0(4) . . . . ?
C20 N6 C19 N5 -176.4(2) . . . . ?
C20 N6 C19 C21 0.4(4) . . . . ?
C21 N7 C24 C23 -0.5(3) . . . . ?
C21 N8 C22 C23 -0.2(4) . . . . ?
C22 N8 C21 N7 0.8(4) . . . . ?
C22 N8 C21 C19 -178.1(2) . . . . ?
C22 C23 C24 N7 1.0(4) . . . . ?
C24 N7 C21 N8 -0.4(3) . . . . ?
C24 N7 C21 C19 178.55(19) . . . . ?
C25 N9 C31 N10 0.9(3) . . . . ?
C25 N9 C31 C33 -175.02(19) . . . . ?
C25 C26 C27 C28 -0.6(5) . . . . ?
C26 C25 C30 N10 -178.5(2) . . . . ?
C26 C25 C30 C29 -1.5(4) . . . . ?
C26 C27 C28 C29 -1.4(5) . . . . ?
C27 C28 C29 C30 2.0(5) . . . . ?
C28 C29 C30 N10 175.7(3) . . . . ?
C28 C29 C30 C25 -0.5(4) . . . . ?
C30 N10 C31 N9 -1.4(3) . . . . ?
C30 N10 C31 C33 174.1(2) . . . . ?
C30 C25 C26 C27 2.0(4) . . . . ?
C31 N9 C25 C26 177.3(3) . . . . ?
C31 N9 C25 C30 -0.1(2) . . . . ?
C31 N10 C30 C25 1.2(2) . . . . ?
C31 N10 C30 C29 -175.4(3) . . . . ?
C32 N10 C30 C25 -179.2(2) . . . . ?
C32 N10 C30 C29 4.1(4) . . . . ?
C32 N10 C31 N9 179.1(2) . . . . ?
C32 N10 C31 C33 -5.4(4) . . . . ?
C33 N11 C36 C35 1.0(4) . . . . ?
C33 N12 C34 C35 -0.2(4) . . . . ?
C34 N12 C33 N11 1.2(4) . . . . ?
C34 N12 C33 C31 -179.6(2) . . . . ?
C34 C35 C36 N11 -0.1(4) . . . . ?
C36 N11 C33 N12 -1.6(3) . . . . ?
C36 N11 C33 C31 179.2(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9993 -0.0002 -0.0022 -0.1543 -0.0264 0.0448
0.9993 0.0002 0.0022 0.1543 0.0264 -0.0448
0.0018 2.9941 -4.9954 -0.1630 -0.0474 -0.4206
-0.0002 -0.9990 0.0002 0.0191 -0.0570 0.0321
0.0002 0.9990 -0.0002 -0.0191 0.0570 -0.0321
0.0000 0.9996 0.9988 0.0021 0.1007 0.0328
0.0002 -0.0006 -0.9990 -0.0212 -0.0437 -0.0649
-0.0009 -0.9972 2.9971 0.0825 0.0741 0.2267
