#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:08:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179441 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/38/4333856.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_4333856
loop_
_publ_author_name
'Hamid Khaledi'
'Marilyn M. Olmstead'
'Hapipah Mohd Ali'
'Noel F. Thomas'
_publ_section_title
;
 Indolenine meso-Substituted Dibenzotetraaza[14]annulene and Its
 Coordination Chemistry toward the Transition Metal Ions MnIII, FeIII,
 CoII, NiII, CuII, and PdII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1926
_journal_page_last               1941
_journal_paper_doi               10.1021/ic302150j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C38 H32 N6 Ni'
_chemical_formula_sum            'C38 H32 N6 Ni'
_chemical_formula_weight         631.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.360(11)
_cell_angle_beta                 85.388(7)
_cell_angle_gamma                87.456(7)
_cell_formula_units_Z            2
_cell_length_a                   6.896(5)
_cell_length_b                   14.223(10)
_cell_length_c                   14.999(12)
_cell_measurement_reflns_used    5497
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      3.152
_cell_measurement_theta_min      32.261
_cell_volume                     1452.5(19)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'Apex2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART Apex II'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Beamline 11.3.1, ALS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14648
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.9587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0433
_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)+(0.0663P)²+1.4491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                4339
_reflns_number_total             5229
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302150j_si_002_04.cif
_cod_data_source_block           NiL
_cod_database_code               4333856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.5000 0.5000 0.5000 0.01612(15) Uani 1 2 d S
N1 N 0.5771(4) 0.24503(18) 0.25758(17) 0.0204(5) Uani 1 1 d .
N2 N 0.5149(3) 0.54367(17) 0.37672(16) 0.0187(5) Uani 1 1 d .
N3 N 0.5218(3) 0.37266(17) 0.48361(16) 0.0180(5) Uani 1 1 d .
C1 C 0.5927(4) 0.2119(2) 0.1723(2) 0.0214(6) Uani 1 1 d .
C2 C 0.6050(5) 0.1182(2) 0.1563(2) 0.0252(7) Uani 1 1 d .
H2 H 0.6042 0.0677 0.2047 0.030 Uiso 1 1 calc R
C3 C 0.6186(5) 0.1005(2) 0.0669(2) 0.0303(8) Uani 1 1 d .
H3 H 0.6263 0.0368 0.0539 0.036 Uiso 1 1 calc R
C4 C 0.6212(5) 0.1745(3) -0.0035(2) 0.0318(8) Uani 1 1 d .
H4 H 0.6307 0.1607 -0.0640 0.038 Uiso 1 1 calc R
C5 C 0.6101(5) 0.2689(2) 0.0131(2) 0.0284(7) Uani 1 1 d .
H5 H 0.6120 0.3195 -0.0351 0.034 Uiso 1 1 calc R
C6 C 0.5963(4) 0.2866(2) 0.1020(2) 0.0217(6) Uani 1 1 d .
C7 C 0.5805(4) 0.3782(2) 0.14260(19) 0.0193(6) Uani 1 1 d .
C8 C 0.7647(4) 0.4358(2) 0.1136(2) 0.0244(7) Uani 1 1 d .
H8A H 0.8788 0.3998 0.1366 0.037 Uiso 1 1 calc R
H8B H 0.7511 0.4964 0.1381 0.037 Uiso 1 1 calc R
H8C H 0.7811 0.4477 0.0476 0.037 Uiso 1 1 calc R
C9 C 0.3942(4) 0.4344(2) 0.1154(2) 0.0243(7) Uani 1 1 d .
H9A H 0.3956 0.4462 0.0495 0.036 Uiso 1 1 calc R
H9B H 0.3880 0.4952 0.1398 0.036 Uiso 1 1 calc R
H9C H 0.2802 0.3979 0.1396 0.036 Uiso 1 1 calc R
C10 C 0.5688(4) 0.3371(2) 0.2436(2) 0.0190(6) Uani 1 1 d .
C11 C 0.5488(4) 0.3924(2) 0.32022(19) 0.0186(6) Uani 1 1 d .
C12 C 0.5358(4) 0.4908(2) 0.31001(19) 0.0191(6) Uani 1 1 d .
H12 H 0.5425 0.5230 0.2502 0.023 Uiso 1 1 calc R
C13 C 0.5024(4) 0.6439(2) 0.3569(2) 0.0180(6) Uani 1 1 d .
C14 C 0.5065(4) 0.6975(2) 0.2726(2) 0.0225(6) Uani 1 1 d .
H14 H 0.5162 0.6668 0.2199 0.027 Uiso 1 1 calc R
C15 C 0.4964(5) 0.7952(2) 0.2649(2) 0.0261(7) Uani 1 1 d .
H15 H 0.5004 0.8312 0.2068 0.031 Uiso 1 1 calc R
C16 C 0.4803(5) 0.8418(2) 0.3408(2) 0.0246(7) Uani 1 1 d .
H16 H 0.4746 0.9091 0.3348 0.029 Uiso 1 1 calc R
C17 C 0.4727(4) 0.7888(2) 0.4257(2) 0.0216(6) Uani 1 1 d .
H17 H 0.4605 0.8202 0.4781 0.026 Uiso 1 1 calc R
C18 C 0.4830(4) 0.6907(2) 0.43446(19) 0.0186(6) Uani 1 1 d .
C19 C 0.5413(4) 0.3381(2) 0.4062(2) 0.0197(6) Uani 1 1 d .
H19 H 0.5512 0.2711 0.4084 0.024 Uiso 1 1 calc R
Ni2 Ni 0.0000 0.5000 0.5000 0.01536(15) Uani 1 2 d S
N4 N 0.0746(4) 0.27370(17) 0.23454(17) 0.0197(5) Uani 1 1 d .
N5 N 0.0160(3) 0.36844(17) 0.53096(16) 0.0173(5) Uani 1 1 d .
N6 N 0.0235(3) 0.49387(17) 0.37695(16) 0.0172(5) Uani 1 1 d .
C20 C 0.0906(4) 0.1900(2) 0.1931(2) 0.0194(6) Uani 1 1 d .
C21 C 0.1051(4) 0.1855(2) 0.1010(2) 0.0236(7) Uani 1 1 d .
H21 H 0.1058 0.2415 0.0587 0.028 Uiso 1 1 calc R
C22 C 0.1186(5) 0.0957(2) 0.0727(2) 0.0259(7) Uani 1 1 d .
H22 H 0.1270 0.0902 0.0100 0.031 Uiso 1 1 calc R
C23 C 0.1198(5) 0.0147(2) 0.1348(2) 0.0275(7) Uani 1 1 d .
H23 H 0.1303 -0.0458 0.1141 0.033 Uiso 1 1 calc R
C24 C 0.1059(5) 0.0203(2) 0.2278(2) 0.0240(7) Uani 1 1 d .
H24 H 0.1072 -0.0356 0.2703 0.029 Uiso 1 1 calc R
C25 C 0.0904(4) 0.1086(2) 0.2560(2) 0.0194(6) Uani 1 1 d .
C26 C 0.0713(4) 0.1397(2) 0.34905(19) 0.0188(6) Uani 1 1 d .
C27 C 0.2496(4) 0.1051(2) 0.4011(2) 0.0233(6) Uani 1 1 d .
H27A H 0.2592 0.0355 0.4083 0.035 Uiso 1 1 calc R
H27B H 0.2357 0.1268 0.4607 0.035 Uiso 1 1 calc R
H27C H 0.3677 0.1307 0.3676 0.035 Uiso 1 1 calc R
C28 C -0.1177(4) 0.1029(2) 0.4013(2) 0.0237(7) Uani 1 1 d .
H28A H -0.2301 0.1310 0.3700 0.035 Uiso 1 1 calc R
H28B H -0.1253 0.1207 0.4624 0.035 Uiso 1 1 calc R
H28C H -0.1181 0.0337 0.4046 0.035 Uiso 1 1 calc R
C29 C 0.0634(4) 0.2484(2) 0.3213(2) 0.0188(6) Uani 1 1 d .
C30 C 0.0452(4) 0.3227(2) 0.3815(2) 0.0193(6) Uani 1 1 d .
C31 C 0.0325(4) 0.3031(2) 0.4751(2) 0.0189(6) Uani 1 1 d .
H31 H 0.0359 0.2384 0.5008 0.023 Uiso 1 1 calc R
C32 C 0.0057(4) 0.3401(2) 0.62583(19) 0.0179(6) Uani 1 1 d .
C33 C 0.0213(4) 0.2475(2) 0.6696(2) 0.0228(6) Uani 1 1 d .
H33 H 0.0388 0.1957 0.6354 0.027 Uiso 1 1 calc R
C34 C 0.0111(5) 0.2314(2) 0.7623(2) 0.0250(7) Uani 1 1 d .
H34 H 0.0219 0.1682 0.7919 0.030 Uiso 1 1 calc R
C35 C -0.0149(4) 0.3066(2) 0.8133(2) 0.0234(7) Uani 1 1 d .
H35 H -0.0227 0.2949 0.8773 0.028 Uiso 1 1 calc R
C36 C -0.0293(4) 0.3986(2) 0.7701(2) 0.0209(6) Uani 1 1 d .
H36 H -0.0475 0.4502 0.8045 0.025 Uiso 1 1 calc R
C37 C -0.0173(4) 0.4156(2) 0.6770(2) 0.0178(6) Uani 1 1 d .
C38 C 0.0397(4) 0.4165(2) 0.3377(2) 0.0193(6) Uani 1 1 d .
H38 H 0.0487 0.4246 0.2736 0.023 Uiso 1 1 calc 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'
Ni Ni 0.3279 1.2288 '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
N3 Ni1 N3 180.000(1) . 2_666 ?
N3 Ni1 N2 85.73(11) . 2_666 y
N3 Ni1 N2 94.27(11) 2_666 2_666 ?
N3 Ni1 N2 94.27(11) . . ?
N3 Ni1 N2 85.73(11) 2_666 . ?
N2 Ni1 N2 179.999(1) 2_666 . ?
C10 N1 C1 107.6(3) . . ?
C12 N2 C13 119.8(3) . . y
C12 N2 Ni1 126.5(2) . . ?
C13 N2 Ni1 113.74(19) . . ?
C19 N3 C18 119.4(3) . 2_666 y
C19 N3 Ni1 126.7(2) . . ?
C18 N3 Ni1 113.88(19) 2_666 . ?
C2 C1 C6 121.7(3) . . ?
C2 C1 N1 126.6(3) . . ?
C6 C1 N1 111.7(3) . . ?
C1 C2 C3 117.6(3) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 121.0(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 118.0(3) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 C1 120.6(3) . . ?
C5 C6 C7 131.4(3) . . ?
C1 C6 C7 108.0(3) . . ?
C6 C7 C9 110.0(2) . . ?
C6 C7 C8 109.9(2) . . ?
C9 C7 C8 111.9(2) . . ?
C6 C7 C10 99.1(2) . . ?
C9 C7 C10 112.6(2) . . ?
C8 C7 C10 112.7(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 120.3(3) . . ?
N1 C10 C7 113.7(3) . . ?
C11 C10 C7 126.0(3) . . ?
C12 C11 C19 121.6(3) . . y
C12 C11 C10 123.2(3) . . ?
C19 C11 C10 115.1(3) . . ?
N2 C12 C11 125.4(3) . . y
N2 C12 H12 117.3 . . ?
C11 C12 H12 117.3 . . ?
C14 C13 C18 119.1(3) . . ?
C14 C13 N2 127.6(3) . . ?
C18 C13 N2 113.4(3) . . y
C15 C14 C13 120.3(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 121.0(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C13 120.0(3) . . ?
C17 C18 N3 126.8(3) . 2_666 ?
C13 C18 N3 113.3(3) . 2_666 y
N3 C19 C11 125.4(3) . . y
N3 C19 H19 117.3 . . ?
C11 C19 H19 117.3 . . ?
N6 Ni2 N6 179.999(1) . 2_566 ?
N6 Ni2 N5 85.92(10) . 2_566 ?
N6 Ni2 N5 94.08(10) 2_566 2_566 ?
N6 Ni2 N5 94.08(10) . . ?
N6 Ni2 N5 85.92(10) 2_566 . ?
N5 Ni2 N5 180.00(4) 2_566 . ?
C29 N4 C20 107.3(2) . . ?
C31 N5 C32 119.8(2) . . ?
C31 N5 Ni2 127.1(2) . . ?
C32 N5 Ni2 113.11(18) . . ?
C38 N6 C37 119.6(3) . 2_566 ?
C38 N6 Ni2 126.5(2) . . ?
C37 N6 Ni2 113.92(19) 2_566 . ?
C21 C20 C25 121.9(3) . . ?
C21 C20 N4 125.9(3) . . ?
C25 C20 N4 112.2(3) . . ?
C20 C21 C22 117.6(3) . . ?
C20 C21 H21 121.2 . . ?
C22 C21 H21 121.2 . . ?
C23 C22 C21 120.7(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 121.1(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 118.3(3) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C24 C25 C20 120.3(3) . . ?
C24 C25 C26 132.0(3) . . ?
C20 C25 C26 107.7(2) . . ?
C25 C26 C27 110.7(2) . . ?
C25 C26 C28 110.2(2) . . ?
C27 C26 C28 110.9(3) . . ?
C25 C26 C29 98.9(2) . . ?
C27 C26 C29 112.9(2) . . ?
C28 C26 C29 112.8(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 C30 118.8(3) . . ?
N4 C29 C26 113.9(2) . . ?
C30 C29 C26 127.3(3) . . ?
C31 C30 C38 121.4(3) . . ?
C31 C30 C29 123.3(3) . . ?
C38 C30 C29 115.3(3) . . ?
N5 C31 C30 124.7(3) . . ?
N5 C31 H31 117.7 . . ?
C30 C31 H31 117.7 . . ?
C33 C32 C37 119.4(3) . . ?
C33 C32 N5 126.6(3) . . ?
C37 C32 N5 113.9(3) . . ?
C34 C33 C32 119.8(3) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.7(3) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C36 C35 C34 119.6(3) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C32 120.3(3) . . ?
C36 C37 N6 126.6(3) . 2_566 ?
C32 C37 N6 113.1(3) . 2_566 ?
N6 C38 C30 126.2(3) . . ?
N6 C38 H38 116.9 . . ?
C30 C38 H38 116.9 . . ?
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 N3 1.858(3) . y
Ni1 N3 1.858(3) 2_666 ?
Ni1 N2 1.867(3) 2_666 ?
Ni1 N2 1.867(3) . y
N1 C10 1.297(4) . y
N1 C1 1.416(4) . ?
N2 C12 1.325(4) . y
N2 C13 1.417(4) . y
N3 C19 1.314(4) . y
N3 C18 1.423(4) 2_666 y
C1 C2 1.382(4) . ?
C1 C6 1.394(4) . ?
C2 C3 1.393(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.506(4) . ?
C7 C9 1.538(4) . ?
C7 C8 1.544(4) . ?
C7 C10 1.547(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.471(4) . y
C11 C12 1.387(4) . y
C11 C19 1.411(4) . y
C12 H12 0.9500 . ?
C13 C14 1.386(4) . ?
C13 C18 1.409(4) . ?
C14 C15 1.378(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(4) . ?
C17 H17 0.9500 . ?
C18 N3 1.423(4) 2_666 ?
C19 H19 0.9500 . ?
Ni2 N6 1.853(3) . ?
Ni2 N6 1.853(3) 2_566 ?
Ni2 N5 1.868(3) 2_566 ?
Ni2 N5 1.868(3) . ?
N4 C29 1.301(4) . ?
N4 C20 1.411(4) . ?
N5 C31 1.327(4) . ?
N5 C32 1.424(4) . ?
N6 C38 1.311(4) . ?
N6 C37 1.427(4) 2_566 ?
C20 C21 1.387(4) . ?
C20 C25 1.392(4) . ?
C21 C22 1.395(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.404(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.514(4) . ?
C26 C27 1.538(4) . ?
C26 C28 1.541(4) . ?
C26 C29 1.546(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.473(4) . ?
C30 C31 1.391(4) . ?
C30 C38 1.407(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.395(4) . ?
C32 C37 1.398(4) . ?
C33 C34 1.376(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.393(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.382(4) . ?
C36 H36 0.9500 . ?
C37 N6 1.427(4) 2_566 ?
C38 H38 0.9500 . ?
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
C8 H8A N4 0.98 2.57 3.500(4) 158.4 1_655
C9 H9C N4 0.98 2.53 3.465(4) 160.2 .
C27 H27C N1 0.98 2.56 3.490(4) 157.9 .
C28 H28A N1 0.98 2.59 3.515(4) 158.3 1_455
#BEGIN Loops that were not found in dictionaries:
loop_
_shelx_res_file
;
TITL NiL in P-1 ALS data
CELL 0.77490   6.896  14.223  14.999  82.360  85.388  87.456
ZERR    2.00   0.005   0.010   0.012   0.011   0.007   0.007
LATT 1
SFAC C  H  N  Ni
DISP NI 0.32791 1.22882
UNIT 76 64 12 2
L.S. 12
BOND $H
ACTA
OMIT 0 -3 4
size 0.06 0.04 0.008
temp -123
WGHT    0.066300    1.449100
BASF   0.21188
FVAR      10.82306
NI1   4    0.500000    0.500000    0.500000    10.50000    0.01919    0.01679 =
         0.01279   -0.00390   -0.00083    0.00033
N1    3    0.577071    0.245034    0.257582    11.00000    0.02014    0.02343 =
         0.01861   -0.00687   -0.00125    0.00084
N2    3    0.514910    0.543666    0.376717    11.00000    0.01819    0.02058 =
         0.01788   -0.00357   -0.00241   -0.00085
N3    3    0.521775    0.372659    0.483612    11.00000    0.01741    0.02168 =
         0.01532   -0.00332   -0.00222    0.00034
C1    1    0.592656    0.211850    0.172294    11.00000    0.01919    0.02550 =
         0.02074   -0.00888    0.00004    0.00128
C2    1    0.605009    0.118204    0.156343    11.00000    0.02456    0.02384 =
         0.02830   -0.00808   -0.00178   -0.00014
AFIX  43
H2    2    0.604233    0.067705    0.204663    11.00000   -1.20000
AFIX   0
C3    1    0.618635    0.100522    0.066894    11.00000    0.02595    0.03305 =
         0.03557   -0.02042   -0.00163    0.00406
AFIX  43
H3    2    0.626283    0.036838    0.053872    11.00000   -1.20000
AFIX   0
C4    1    0.621213    0.174512   -0.003514    11.00000    0.02928    0.04628 =
         0.02358   -0.01893   -0.00351    0.00420
AFIX  43
H4    2    0.630685    0.160678   -0.063988    11.00000   -1.20000
AFIX   0
C5    1    0.610113    0.268899    0.013112    11.00000    0.02961    0.03491 =
         0.02136   -0.00815   -0.00249    0.00435
AFIX  43
H5    2    0.612001    0.319504   -0.035124    11.00000   -1.20000
AFIX   0
C6    1    0.596272    0.286585    0.101955    11.00000    0.01596    0.02921 =
         0.02084   -0.00776   -0.00111    0.00196
C7    1    0.580506    0.378151    0.142598    11.00000    0.02035    0.02085 =
         0.01680   -0.00385   -0.00006    0.00161
C8    1    0.764692    0.435800    0.113582    11.00000    0.02292    0.02618 =
         0.02362   -0.00183   -0.00119   -0.00035
AFIX 137
H8A   2    0.878759    0.399848    0.136594    11.00000   -1.50000
H8B   2    0.751108    0.496450    0.138145    11.00000   -1.50000
H8C   2    0.781121    0.447697    0.047587    11.00000   -1.50000
AFIX   0
C9    1    0.394177    0.434449    0.115436    11.00000    0.02365    0.02611 =
         0.02196    0.00051   -0.00235    0.00140
AFIX 137
H9A   2    0.395583    0.446173    0.049511    11.00000   -1.50000
H9B   2    0.387993    0.495183    0.139848    11.00000   -1.50000
H9C   2    0.280199    0.397872    0.139638    11.00000   -1.50000
AFIX   0
C10   1    0.568825    0.337056    0.243618    11.00000    0.01561    0.02346 =
         0.01873   -0.00549   -0.00203    0.00162
C11   1    0.548771    0.392432    0.320218    11.00000    0.01789    0.02279 =
         0.01612   -0.00628   -0.00094   -0.00116
C12   1    0.535806    0.490803    0.310009    11.00000    0.01966    0.02287 =
         0.01499   -0.00277   -0.00154   -0.00124
AFIX  43
H12   2    0.542466    0.522956    0.250186    11.00000   -1.20000
AFIX   0
C13   1    0.502420    0.643911    0.356914    11.00000    0.01373    0.02059 =
         0.02041   -0.00568   -0.00160    0.00132
C14   1    0.506458    0.697520    0.272608    11.00000    0.02519    0.02504 =
         0.01814   -0.00547   -0.00258   -0.00032
AFIX  43
H14   2    0.516234    0.666769    0.219864    11.00000   -1.20000
AFIX   0
C15   1    0.496357    0.795246    0.264929    11.00000    0.03247    0.02714 =
         0.01854    0.00006   -0.00526   -0.00135
AFIX  43
H15   2    0.500450    0.831212    0.206753    11.00000   -1.20000
AFIX   0
C16   1    0.480326    0.841762    0.340795    11.00000    0.02817    0.01965 =
         0.02581   -0.00326   -0.00377    0.00387
AFIX  43
H16   2    0.474574    0.909146    0.334825    11.00000   -1.20000
AFIX   0
C17   1    0.472749    0.788811    0.425731    11.00000    0.02313    0.02274 =
         0.01966   -0.00611   -0.00170    0.00037
AFIX  43
H17   2    0.460477    0.820167    0.478114    11.00000   -1.20000
AFIX   0
C18   1    0.482974    0.690678    0.434457    11.00000    0.01471    0.02504 =
         0.01623   -0.00377   -0.00171    0.00073
C19   1    0.541302    0.338150    0.406220    11.00000    0.01843    0.01954 =
         0.02155   -0.00540   -0.00022    0.00180
AFIX  43
H19   2    0.551216    0.271066    0.408358    11.00000   -1.20000
AFIX   0
NI2   4    0.000000    0.500000    0.500000    10.50000    0.01883    0.01278 =
         0.01504   -0.00454   -0.00067    0.00019
N4    3    0.074600    0.273700    0.234536    11.00000    0.02041    0.01827 =
         0.02087   -0.00622    0.00065    0.00088
N5    3    0.016031    0.368437    0.530960    11.00000    0.01750    0.01710 =
         0.01760   -0.00453   -0.00001   -0.00001
N6    3    0.023494    0.493867    0.376953    11.00000    0.01768    0.01548 =
         0.01822   -0.00249   -0.00068   -0.00016
C20   1    0.090565    0.189984    0.193109    11.00000    0.02040    0.01859 =
         0.02052   -0.00766   -0.00213    0.00274
C21   1    0.105092    0.185480    0.100974    11.00000    0.02415    0.02651 =
         0.02062   -0.00587   -0.00028   -0.00172
AFIX  43
H21   2    0.105834    0.241494    0.058688    11.00000   -1.20000
AFIX   0
C22   1    0.118571    0.095709    0.072666    11.00000    0.02820    0.03208 =
         0.01984   -0.01367    0.00027   -0.00072
AFIX  43
H22   2    0.126971    0.090209    0.010029    11.00000   -1.20000
AFIX   0
C23   1    0.119836    0.014688    0.134754    11.00000    0.03000    0.02367 =
         0.03114   -0.01448    0.00106    0.00079
AFIX  43
H23   2    0.130305   -0.045785    0.114115    11.00000   -1.20000
AFIX   0
C24   1    0.105909    0.020268    0.227804    11.00000    0.02898    0.01977 =
         0.02345   -0.00428   -0.00147    0.00001
AFIX  43
H24   2    0.107178   -0.035594    0.270253    11.00000   -1.20000
AFIX   0
C25   1    0.090388    0.108593    0.255963    11.00000    0.01733    0.02052 =
         0.02117   -0.00747    0.00040    0.00036
C26   1    0.071279    0.139715    0.349049    11.00000    0.02274    0.01686 =
         0.01788   -0.00723   -0.00114    0.00014
C27   1    0.249625    0.105051    0.401146    11.00000    0.02589    0.02019 =
         0.02472   -0.00540   -0.00455    0.00269
AFIX 137
H27A  2    0.259170    0.035540    0.408339    11.00000   -1.50000
H27B  2    0.235715    0.126830    0.460707    11.00000   -1.50000
H27C  2    0.367653    0.130691    0.367593    11.00000   -1.50000
AFIX   0
C28   1   -0.117739    0.102937    0.401268    11.00000    0.02425    0.02174 =
         0.02523   -0.00537    0.00103   -0.00177
AFIX 137
H28A  2   -0.230080    0.131011    0.370023    11.00000   -1.50000
H28B  2   -0.125286    0.120743    0.462397    11.00000   -1.50000
H28C  2   -0.118085    0.033663    0.404600    11.00000   -1.50000
AFIX   0
C29   1    0.063396    0.248363    0.321340    11.00000    0.01729    0.01842 =
         0.02177   -0.00614   -0.00130   -0.00070
C30   1    0.045192    0.322695    0.381489    11.00000    0.01959    0.01761 =
         0.02199   -0.00768   -0.00247    0.00093
C31   1    0.032534    0.303146    0.475079    11.00000    0.02182    0.01324 =
         0.02221   -0.00365   -0.00313   -0.00137
AFIX  43
H31   2    0.035949    0.238411    0.500836    11.00000   -1.20000
AFIX   0
C32   1    0.005738    0.340053    0.625831    11.00000    0.01407    0.02092 =
         0.01885   -0.00253   -0.00111   -0.00190
C33   1    0.021266    0.247474    0.669562    11.00000    0.02785    0.01645 =
         0.02528   -0.00656   -0.00176   -0.00242
AFIX  43
H33   2    0.038841    0.195664    0.635413    11.00000   -1.20000
AFIX   0
C34   1    0.011064    0.231360    0.762321    11.00000    0.03237    0.01639 =
         0.02599   -0.00051   -0.00352   -0.00340
AFIX  43
H34   2    0.021855    0.168222    0.791927    11.00000   -1.20000
AFIX   0
C35   1   -0.014917    0.306633    0.813276    11.00000    0.02602    0.02723 =
         0.01726   -0.00332   -0.00085   -0.00493
AFIX  43
H35   2   -0.022707    0.294882    0.877289    11.00000   -1.20000
AFIX   0
C36   1   -0.029307    0.398619    0.770075    11.00000    0.02103    0.02227 =
         0.02035   -0.00629   -0.00161   -0.00104
AFIX  43
H36   2   -0.047496    0.450182    0.804512    11.00000   -1.20000
AFIX   0
C37   1   -0.017280    0.415647    0.676955    11.00000    0.01481    0.01663 =
         0.02218   -0.00294   -0.00160   -0.00064
C38   1    0.039729    0.416547    0.337700    11.00000    0.01919    0.02332 =
         0.01606   -0.00582   -0.00029   -0.00137
AFIX  43
H38   2    0.048651    0.424640    0.273621    11.00000   -1.20000
 
HKLF 5
 
REM  mn2069 in P-1 ALS data
REM R1 =  0.0433 for   4339 Fo > 4sig(Fo)  and  0.0532 for all   5229 data
REM    414 parameters refined using      0 restraints
 
END  
     
WGHT      0.0663      1.4392 
REM Highest difference peak  0.649,  deepest hole -0.372,  1-sigma level  0.074
Q1    1   0.0740  0.5418  0.5448  11.00000  0.05    0.65
Q2    1   0.4247  0.4566  0.4562  11.00000  0.05    0.61
Q3    1   0.1218  0.4975  0.7568  11.00000  0.05    0.58
Q4    1   0.3643  0.5013  0.2503  11.00000  0.05    0.57
;
#END Loops that were not found in dictionaries
