#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:02:31 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/69/7716914.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_7716914
loop_
_publ_author_name
'Álvarez-Miguel, Lucía'
'Del Carmen-Rodríguez, Clara'
'Valle, María'
'Álvarez, Celedonio M'
'Martín-Álvarez, José M'
'García-Rodríguez, Raúl'
'Miguel, Daniel'
_publ_section_title
;
 Synthesis and reactivity of air stable Ni(II) complexes with isocyanides
 and dialkyldithiophosphate ligands: acyclic diaminocarbene formation.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15101
_journal_page_last               15112
_journal_paper_doi               10.1039/d4dt01915f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C42 H52 N6 Ni2 O4 P2 S4'
_chemical_formula_sum            'C46 H52 N6 Ni2 O4 P2 S4'
_chemical_formula_weight         1060.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.398(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8519(11)
_cell_length_b                   12.9097(15)
_cell_length_c                   25.918(2)
_cell_measurement_reflns_used    1944
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.0350
_cell_measurement_theta_min      2.4250
_cell_volume                     5180.3(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  92.00   1.00   80.50    --   11.75-179.00  60.00   48
  2  ω    -68.00  36.00   1.00   80.50    --   11.75 -19.00  30.00  104
  3  ω    -18.00  38.00   1.00   80.50    --   11.75  77.00  60.00   56
;
_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      0.0027175000
_diffrn_orient_matrix_UB_12      -0.0496297000
_diffrn_orient_matrix_UB_13      -0.0113945000
_diffrn_orient_matrix_UB_21      -0.0263016000
_diffrn_orient_matrix_UB_22      -0.0207995000
_diffrn_orient_matrix_UB_23      0.0164118000
_diffrn_orient_matrix_UB_31      -0.0373317000
_diffrn_orient_matrix_UB_32      0.0110483000
_diffrn_orient_matrix_UB_33      -0.0197010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.736
_diffrn_reflns_theta_max         24.736
_diffrn_reflns_theta_min         2.054
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4420
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0853P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2225
_reflns_number_total             4420
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01915f2.cif
_cod_data_source_block           lam511a
_cod_depositor_comments
'Adding full bibliography for 7716902--7716918.cif.'
_cod_original_cell_volume        5180.2(8)
_cod_database_code               7716914
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H52 N6 O4 P2 S4 Ni2'
_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 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.717
_oxdiff_exptl_absorpt_empirical_full_min 0.662
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.63736(5) 0.33415(6) 0.61271(3) 0.0618(3) Uani 1 1 d . . . . .
S1 S 0.73248(11) 0.46065(14) 0.61784(8) 0.0763(6) Uani 1 1 d . . . . .
S2 S 0.74684(10) 0.22319(15) 0.63205(8) 0.0769(6) Uani 1 1 d . . . . .
P1 P 0.82463(11) 0.34857(15) 0.63914(8) 0.0699(6) Uani 1 1 d . . . . .
O1 O 0.8969(3) 0.3478(4) 0.6117(2) 0.0887(15) Uani 1 1 d . . . . .
O2 O 0.8711(3) 0.3642(5) 0.6999(2) 0.1090(19) Uani 1 1 d . . . . .
N1 N 0.5130(3) 0.4827(5) 0.6301(2) 0.0724(18) Uani 1 1 d . . . . .
H1 H 0.480(4) 0.532(6) 0.624(3) 0.087 Uiso 1 1 d . U . . .
N2 N 0.5200(4) 0.1532(6) 0.5846(3) 0.097(2) Uani 1 1 d . . . . .
N3 N 0.5025(3) 0.4354(5) 0.5434(2) 0.0764(17) Uani 1 1 d . . . . .
C1 C 0.5421(4) 0.4288(5) 0.5940(3) 0.0603(17) Uani 1 1 d . . . . .
C2 C 0.5633(5) 0.2238(6) 0.5985(3) 0.074(2) Uani 1 1 d . . . . .
C11 C 0.5492(5) 0.4787(7) 0.6858(3) 0.085(2) Uani 1 1 d . . . . .
C12 C 0.5297(8) 0.4010(11) 0.7166(4) 0.129(4) Uani 1 1 d . . . . .
C13 C 0.5688(11) 0.4009(14) 0.7708(6) 0.171(7) Uani 1 1 d . . . . .
H13 H 0.5592 0.3459 0.7920 0.206 Uiso 1 1 calc R U . . .
C14 C 0.6194(12) 0.4793(16) 0.7919(6) 0.180(9) Uani 1 1 d . . . . .
H14 H 0.6432 0.4789 0.8280 0.216 Uiso 1 1 calc R U . . .
C15 C 0.6378(7) 0.5627(12) 0.7610(5) 0.151(5) Uani 1 1 d . . . . .
H15 H 0.6738 0.6164 0.7763 0.182 Uiso 1 1 calc R U . . .
C16 C 0.6011(6) 0.5629(9) 0.7072(3) 0.096(3) Uani 1 1 d . . . . .
C17 C 0.4647(8) 0.3208(9) 0.6954(5) 0.167(5) Uani 1 1 d . . . . .
H17A H 0.4663 0.3067 0.6592 0.251 Uiso 1 1 calc R U . . .
H17B H 0.4082 0.3453 0.6973 0.251 Uiso 1 1 calc R U . . .
H17C H 0.4773 0.2586 0.7158 0.251 Uiso 1 1 calc R U . . .
C18 C 0.6188(6) 0.6540(8) 0.6761(4) 0.125(3) Uani 1 1 d . . . . .
H18A H 0.6457 0.6313 0.6483 0.188 Uiso 1 1 calc R U . . .
H18B H 0.6566 0.7009 0.6989 0.188 Uiso 1 1 calc R U . . .
H18C H 0.5655 0.6885 0.6612 0.188 Uiso 1 1 calc R U . . .
C20 C 0.8241(7) 0.3727(10) 0.7411(3) 0.169(5) Uani 1 1 d . . . . .
H20A H 0.7661 0.3947 0.7264 0.254 Uiso 1 1 calc R U . . .
H20B H 0.8517 0.4225 0.7668 0.254 Uiso 1 1 calc R U . . .
H20C H 0.8229 0.3066 0.7579 0.254 Uiso 1 1 calc R U . . .
C21 C 0.4713(6) 0.0650(8) 0.5657(4) 0.105(3) Uani 1 1 d . U . . .
C22 C 0.4019(7) 0.0759(10) 0.5222(5) 0.137(4) Uani 1 1 d . U . . .
C23 C 0.3563(7) -0.0165(12) 0.5039(6) 0.165(5) Uani 1 1 d . U . . .
H23 H 0.3105 -0.0147 0.4747 0.198 Uiso 1 1 calc R U . . .
C24 C 0.3811(10) -0.1109(12) 0.5302(7) 0.174(6) Uani 1 1 d . U . . .
H24 H 0.3506 -0.1712 0.5189 0.208 Uiso 1 1 calc R U . . .
C25 C 0.4485(10) -0.1139(10) 0.5716(6) 0.158(4) Uani 1 1 d . U . . .
H25 H 0.4631 -0.1770 0.5885 0.190 Uiso 1 1 calc R U . . .
C26 C 0.4976(7) -0.0274(8) 0.5903(5) 0.117(3) Uani 1 1 d . . . . .
C27 C 0.3764(7) 0.1802(11) 0.4959(6) 0.186(6) Uani 1 1 d . . . . .
H27A H 0.3634 0.2279 0.5215 0.279 Uiso 1 1 calc R U . . .
H27B H 0.3264 0.1716 0.4679 0.279 Uiso 1 1 calc R U . . .
H27C H 0.4233 0.2068 0.4818 0.279 Uiso 1 1 calc R U . . .
C28 C 0.5739(9) -0.0340(9) 0.6322(5) 0.175(5) Uani 1 1 d . . . . .
H28A H 0.6225 -0.0066 0.6201 0.263 Uiso 1 1 calc R U . . .
H28B H 0.5847 -0.1051 0.6423 0.263 Uiso 1 1 calc R U . . .
H28C H 0.5653 0.0053 0.6621 0.263 Uiso 1 1 calc R U . . .
C31 C 0.4253(4) 0.5018(6) 0.5236(3) 0.078(2) Uani 1 1 d . . . . .
H31A H 0.3828 0.4641 0.4979 0.094 Uiso 1 1 calc R U . . .
H31B H 0.3990 0.5221 0.5526 0.094 Uiso 1 1 calc R U . . .
C32 C 0.4544(4) 0.5939(6) 0.4990(2) 0.076(2) Uani 1 1 d . . . . .
H32A H 0.4051 0.6376 0.4848 0.091 Uiso 1 1 calc R U . . .
H32B H 0.4939 0.6334 0.5256 0.091 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 0.0033 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 18 1 0.0392
-12 2 -26 0.0303
21 -6 -8 0.1537
2 -2 -36 0.0433
-1 -18 -1 0.0322
-2 2 36 0.0463
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
S1 Ni1 S2 88.45(7) . . ?
C1 Ni1 S1 92.0(2) . . ?
C1 Ni1 S2 178.4(2) . . ?
C2 Ni1 S1 170.8(2) . . ?
C2 Ni1 S2 88.8(2) . . ?
C2 Ni1 C1 90.5(3) . . ?
P1 S1 Ni1 86.10(9) . . ?
P1 S2 Ni1 86.33(9) . . ?
S2 P1 S1 98.96(10) . . ?
O1 P1 S1 117.3(2) . . ?
O1 P1 S2 118.3(2) . . ?
O1 P1 O2 103.5(3) . . ?
O2 P1 S1 109.1(2) . . ?
O2 P1 S2 109.5(2) . . ?
C20 O2 P1 122.7(6) . . ?
C1 N1 H1 125(5) . . ?
C1 N1 C11 124.5(6) . . ?
C11 N1 H1 109(5) . . ?
C2 N2 C21 176.1(8) . . ?
C1 N3 C31 123.7(5) . . ?
C1 N3 C32 121.7(5) . 5_666 ?
C32 N3 C31 111.8(5) 5_666 . ?
N1 C1 Ni1 122.0(5) . . ?
N1 C1 N3 120.0(5) . . ?
N3 C1 Ni1 118.0(5) . . ?
N2 C2 Ni1 172.6(7) . . ?
C12 C11 N1 121.7(10) . . ?
C12 C11 C16 121.9(10) . . ?
C16 C11 N1 116.3(8) . . ?
C11 C12 C13 118.7(14) . . ?
C11 C12 C17 121.7(10) . . ?
C13 C12 C17 119.5(13) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(18) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.7(17) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.7 . . ?
C16 C15 C14 118.6(14) . . ?
C16 C15 H15 120.7 . . ?
C11 C16 C18 124.2(8) . . ?
C15 C16 C11 118.5(11) . . ?
C15 C16 C18 117.3(12) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 118.5(10) . . ?
C26 C21 N2 116.9(10) . . ?
C26 C21 C22 124.6(11) . . ?
C21 C22 C23 116.0(13) . . ?
C21 C22 C27 122.4(10) . . ?
C23 C22 C27 121.6(12) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(14) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(15) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 118.5 . . ?
C24 C25 C26 123.1(15) . . ?
C26 C25 H25 118.5 . . ?
C21 C26 C25 116.4(12) . . ?
C21 C26 C28 121.5(10) . . ?
C25 C26 C28 122.1(13) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 110.2 . . ?
N3 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 N3 107.7(6) . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
N3 C32 C31 110.9(6) 5_666 . ?
N3 C32 H32A 109.5 5_666 . ?
N3 C32 H32B 109.5 5_666 . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
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 S1 2.207(2) . ?
Ni1 S2 2.2231(18) . ?
Ni1 C1 1.921(6) . ?
Ni1 C2 1.832(8) . ?
S1 P1 2.046(3) . ?
S2 P1 2.019(3) . ?
P1 O1 1.472(5) . ?
P1 O2 1.601(5) . ?
O2 C20 1.434(10) . ?
N1 H1 0.81(7) . ?
N1 C1 1.325(8) . ?
N1 C11 1.436(9) . ?
N2 C2 1.151(9) . ?
N2 C21 1.405(10) . ?
N3 C1 1.331(7) . ?
N3 C31 1.492(8) . ?
N3 C32 1.463(8) 5_666 ?
C11 C12 1.358(13) . ?
C11 C16 1.404(12) . ?
C12 C13 1.407(16) . ?
C12 C17 1.482(15) . ?
C13 H13 0.9300 . ?
C13 C14 1.33(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.41(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.392(13) . ?
C16 C18 1.484(12) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.402(14) . ?
C21 C26 1.374(12) . ?
C22 C23 1.423(15) . ?
C22 C27 1.524(15) . ?
C23 H23 0.9300 . ?
C23 C24 1.410(18) . ?
C24 H24 0.9300 . ?
C24 C25 1.343(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(14) . ?
C26 C28 1.445(14) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.468(10) . ?
C32 N3 1.463(8) 5_666 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
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
S1 P1 O2 C20 52.4(8) . . . . ?
S2 P1 O2 C20 -54.9(8) . . . . ?
O1 P1 O2 C20 178.1(8) . . . . ?
N1 C11 C12 C13 178.8(8) . . . . ?
N1 C11 C12 C17 -5.1(13) . . . . ?
N1 C11 C16 C15 -179.9(7) . . . . ?
N1 C11 C16 C18 1.0(11) . . . . ?
N2 C21 C22 C23 178.3(9) . . . . ?
N2 C21 C22 C27 -1.6(15) . . . . ?
N2 C21 C26 C25 179.4(8) . . . . ?
N2 C21 C26 C28 -2.5(15) . . . . ?
N3 C31 C32 N3 57.4(7) . . . 5_666 ?
C1 N1 C11 C12 -80.7(10) . . . . ?
C1 N1 C11 C16 103.4(9) . . . . ?
C1 N3 C31 C32 103.5(7) . . . . ?
C11 N1 C1 Ni1 1.4(10) . . . . ?
C11 N1 C1 N3 177.9(7) . . . . ?
C11 C12 C13 C14 4.3(19) . . . . ?
C12 C11 C16 C15 4.2(12) . . . . ?
C12 C11 C16 C18 -174.9(8) . . . . ?
C12 C13 C14 C15 -2(2) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C11 -1.7(14) . . . . ?
C14 C15 C16 C18 177.5(11) . . . . ?
C16 C11 C12 C13 -5.5(13) . . . . ?
C16 C11 C12 C17 170.6(8) . . . . ?
C17 C12 C13 C14 -171.8(14) . . . . ?
C21 C22 C23 C24 1.5(17) . . . . ?
C22 C21 C26 C25 -3.1(15) . . . . ?
C22 C21 C26 C28 175.0(11) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
C24 C25 C26 C21 3.0(18) . . . . ?
C24 C25 C26 C28 -175.0(13) . . . . ?
C26 C21 C22 C23 0.9(15) . . . . ?
C26 C21 C22 C27 -179.0(11) . . . . ?
C27 C22 C23 C24 -178.6(12) . . . . ?
C31 N3 C1 Ni1 177.1(5) . . . . ?
C31 N3 C1 N1 0.4(10) . . . . ?
C32 N3 C1 Ni1 -23.3(9) 5_666 . . . ?
C32 N3 C1 N1 160.0(7) 5_666 . . . ?
C32 N3 C31 C32 -57.9(8) 5_666 . . . ?
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
1.0397 18.0976 1.0459 -0.9073 -0.3866 0.1405
-11.9139 2.0975 -26.2382 0.1625 -0.1609 0.9849
21.0893 -6.0888 -7.7917 0.4483 -0.5559 -0.7011
2.1671 -1.9534 -36.1172 0.5144 -0.6091 0.6091
-1.0397 -18.0976 -1.0459 0.9073 0.3866 -0.1405
-2.1671 1.9534 36.1172 -0.5144 0.6091 -0.6091
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.238 0.500 130.7 3.7 ?
2 0.250 0.262 0.000 130.7 3.7 ?
3 0.179 0.122 0.741 11.1 0.1 ?
4 0.179 0.378 0.241 11.1 0.1 ?
5 0.250 0.653 0.500 22.2 2.6 ?
6 0.250 0.847 0.000 22.2 2.6 ?
7 0.321 0.122 0.259 11.1 0.1 ?
8 0.321 0.378 0.759 11.1 0.1 ?
9 0.750 0.738 1.000 130.7 3.7 ?
10 0.750 0.762 0.500 130.7 3.7 ?
11 0.679 0.622 0.241 11.1 0.1 ?
12 0.679 0.878 0.741 11.1 0.1 ?
13 0.750 0.153 0.000 22.2 2.6 ?
14 0.750 0.347 0.500 22.2 2.6 ?
15 0.821 0.622 0.759 11.1 0.1 ?
16 0.821 0.878 0.259 11.1 0.1 ?
