# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2011
data_global-cpd2
_journal_name_full CrystEngComm
_journal_coden_cambridge 1350
#TrackingRef '- Compd_2new.cif'
_audit_creation_date 11-05-26
_audit_creation_method CRYSTALS_ver_14.09
_oxford_structure_analysis_title 'monoc in C2/m'
_chemical_name_systematic ?
_chemical_melting_point ?
#looking for refcif
# Check this file using the IUCr facility at:
# http://checkcif.iucr.org/
# The content below is held in the file 'script/refcif.dat'. This is a text
# file which you may edit to reflect local conditions.
# Items which need looking at are represented by a '?'.
# Items for which there are choices are prefixed with 'choose from'.
_publ_contact_letter
;
;
_publ_contact_author_name 'Jean-Pascal Sutter'
_publ_contact_author_address
;
CNRS ; LCC (Laboratoire de Chimie de Coordination),
205 route de Narbonne, F-31077 Toulouse,
France
;
_publ_contact_author_email sutter@lcc-toulouse.fr
_publ_requested_category EO # choose from: FI FM FO CI CM CO AD
_publ_section_title
# Title of paper - generally just the systematic or trivial name
; Oligomeric and polymeric organizations of
potassium salts with compartmental Schiff-base
complexes as ligands
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
# Author 1
# Author 2
# Author 2
# Author 2
'Maliheh Mousavi'
;
CNRS ; LCC (Laboratoire de Chimie de Coordination),
205 route de Narbonne, F-31077 Toulouse,
France
;
;
? # Footnote for author 1
;
V.Bereaua
;
CNRS ; LCC (Laboratoire de Chimie de Coordination),
205 route de Narbonne, F-31077 Toulouse,
France
;
;
? # Footnote 2
;
'Carine Duhayon'
;
CNRS ; LCC (Laboratoire de Chimie de Coordination),
205 route de Narbonne, F-31077 Toulouse,
France
;
;
? # Footnote 2
;
'Jean-Pascal Sutter'
;
CNRS ; LCC (Laboratoire de Chimie de Coordination),
205 route de Narbonne, F-31077 Toulouse,
France
;
;
? # Footnote 2
;
_publ_section_abstract
# Text of the abstract
# (a) The Abstract must be self-contained and comprehensible
# without the rest of the paper. This means no references
# to atom names or to compound numbers; compounds must be
# identified as the title compound, or by name or by some other
# means such as derivatives of each other (e.g. "the
# corresponding ketone").
# (b) The chemical formula of "the title compound" must be given.
# (c) Any crystallographic molecular symmetry should be
# mentioned, and also the presence of more than one molecule
# in the asymmetric unit (i.e. anything other than Z'=1).
;
?
;
_publ_section_related_literature
# Not in version 2.3.1
###############################################################
# Essential references (e.g. to the origin of the material studied, related
# structural studies, and to information supporting the reported structure)
# should be cited in this section, with appropriate very brief explanatory
# text, for example `The synthesis of the complex is described by Jones
# (2001). The anhydrous complex has essentially the same coordination
# geometry (Smith, 2003).' In addition, all references included in the
# supplementary materials, but not elsewhere in the published article,
# should be given here. The simple text `For related literature, see:...'
# may be used, but further details should be provided in the Comment
# section, which forms part of the supplementary material.
###############################################################
;
?
;
_publ_section_comment
# Text of the paper
# Note that atoms are referenced as N2, not N(2) or N~2~
# If text containing () occur within (), the outer ones should be []
# Figures should be referenced as Fig.
;
?
;
_publ_section_acknowledgements # Acknowledgments
;
?
;
_publ_section_figure_captions
# Captions to figures - Start each caption on a new line after a blank line
;
;
_publ_section_exptl_refinement
# Some potentially useful phrases are donated by Bill Clegg:
;
The H atoms were refined with riding constraints.
Hydrogen atoms could not be located on water molecules
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
# Hand-made tables can be put in the cif. The number of columns
# is set in the loop header.
# The contants of each column can either be a piece of text
# without any spaces (eg a number) or other text enclosed in " "
# Remove the leading # in the following example
#geom_extra_table_head_A
#;
#Table 2.
#Molecular parameters deviating most from MOGUL averages
#;
#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
#_geom_extra_tableA_col_4
#
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d"
#N5-C6-C4 129 124 "7 (\%)"
#C3-O10-C2 105 109 "2 (\%)"
#C6-O7 1.25 1.22 ".02 (\%A)"
#
data_1
_database_code_depnum_ccdc_archive 'CCDC 809267'
#TrackingRef '- 1_new_ccdc809267.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 14.1659(4)
_cell_length_b 15.1150(4)
_cell_length_c 15.5887(4)
_cell_angle_alpha 73.0800(10)
_cell_angle_beta 64.4580(10)
_cell_angle_gamma 88.402(2)
_cell_volume 2862.77(14)
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P -1 '
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 1
_chemical_formula_sum 'C102 H114 K3 Mo N20 Ni4 O16 S6 '
_chemical_formula_moiety
'C88 H102 K3 N10 Ni4 O16, C6 Mo N6 S6, 4(C2 H3 N)'
_chemical_compound_source ?
_chemical_formula_weight 2516.62
_cell_measurement_reflns_used 9382
_cell_measurement_theta_min 3
_cell_measurement_theta_max 34
_cell_measurement_temperature 180
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_min 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.250
_exptl_crystal_density_diffrn 1.460
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1301
_exptl_absorpt_coefficient_mu 1.040
# Sheldrick geometric approximatio 0.81 0.81
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min 0.76
_exptl_absorpt_correction_T_max 0.81
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 180
_diffrn_reflns_number 81299
_reflns_number_total 22734
_diffrn_reflns_av_R_equivalents 0.028
# Number of reflections without Friedels Law is 22734
# Number of reflections with Friedels Law is 22734
# Theoretical number of reflections is about 25763
_diffrn_reflns_theta_min 1.417
_diffrn_reflns_theta_max 35.291
_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full 28.586
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 22
_reflns_limit_h_min -20
_reflns_limit_h_max 22
_reflns_limit_k_min -23
_reflns_limit_k_max 23
_reflns_limit_l_min 0
_reflns_limit_l_max 24
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -1.35
_refine_diff_density_max 1.06
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 15993
_refine_ls_number_restraints 0
_refine_ls_number_parameters 667
_oxford_refine_ls_R_factor_ref 0.0366
_refine_ls_wR_factor_ref 0.0386
_refine_ls_goodness_of_fit_ref 1.0000
_refine_ls_shift/su_max 0.0005648
_refine_ls_shift/su_mean 0.0000260
# The values computed from all data
_oxford_reflns_number_all 22698
_refine_ls_R_factor_all 0.0597
_refine_ls_wR_factor_all 0.0809
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 16964
_refine_ls_R_factor_gt 0.0387
_refine_ls_wR_factor_gt 0.0403
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
# WARNING. The IUCr will not accept Unit Weights
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Quasi-Unit weights
W = 1.0 or 1./2F
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Sheldrick, G. M. (2008). Acta Cryst A64, 112-122.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mo1 Mo 0.5000 -0.5000 1.0000 0.0210 1.0000 Uani S . . . . .
Ni1 Ni 0.17494(2) 0.165797(17) 0.762411(19) 0.0197 1.0000 Uani . . . . . .
Ni2 Ni 0.360336(19) 0.038952(17) 0.557184(18) 0.0182 1.0000 Uani . . . . . .
C1 C 0.57853(16) -0.70547(14) 1.00953(16) 0.0260 1.0000 Uani . . . . . .
C2 C 0.2575(2) -0.58493(19) 1.1566(2) 0.0394 1.0000 Uani . . . . . .
C3 C 0.46463(17) -0.48286(14) 0.80240(17) 0.0261 1.0000 Uani . . . . . .
C4 C 0.20504(19) -0.05759(16) 1.12433(17) 0.0298 1.0000 Uani . . . . . .
C5 C 0.24928(16) 0.09018(15) 0.99953(16) 0.0241 1.0000 Uani . . . . . .
C6 C 0.29331(18) 0.12775(17) 1.04646(18) 0.0312 1.0000 Uani . . . . . .
C7 C 0.3449(2) 0.21865(18) 1.0013(2) 0.0381 1.0000 Uani . . . . . .
C8 C 0.3536(2) 0.26921(18) 0.9099(2) 0.0378 1.0000 Uani . . . . . .
C9 C 0.30666(17) 0.23334(15) 0.86130(18) 0.0284 1.0000 Uani . . . . . .
C10 C 0.25243(15) 0.14293(14) 0.90644(15) 0.0224 1.0000 Uani . . . . . .
C11 C 0.32272(18) 0.28670(15) 0.76271(18) 0.0304 1.0000 Uani . . . . . .
C12 C 0.30953(17) 0.32376(15) 0.60933(17) 0.0305 1.0000 Uani . . . . . .
C13 C 0.11601(17) 0.33046(14) 0.66502(17) 0.0289 1.0000 Uani . . . . . .
C14 C 0.06210(16) 0.19183(15) 0.64726(15) 0.0255 1.0000 Uani . . . . . .
C15 C 0.04018(15) 0.09360(15) 0.66846(15) 0.0233 1.0000 Uani . . . . . .
C16 C -0.00808(17) 0.06213(17) 0.61857(16) 0.0300 1.0000 Uani . . . . . .
C17 C -0.04094(18) -0.03022(18) 0.64593(18) 0.0332 1.0000 Uani . . . . . .
C18 C -0.03101(17) -0.09446(16) 0.72657(17) 0.0288 1.0000 Uani . . . . . .
C19 C 0.01431(16) -0.06505(14) 0.77730(15) 0.0232 1.0000 Uani . . . . . .
C20 C 0.05481(15) 0.03001(14) 0.74710(14) 0.0208 1.0000 Uani . . . . . .
C21 C -0.02592(19) -0.21345(15) 0.89979(19) 0.0317 1.0000 Uani . . . . . .
C22 C 0.2317(3) 0.47497(18) 0.6143(3) 0.0529 1.0000 Uani . . . . . .
C23 C 0.2439(2) 0.4015(2) 0.48497(19) 0.0470 1.0000 Uani . . . . . .
C24 C 0.2494(2) -0.32215(16) 0.85941(19) 0.0394 1.0000 Uani . . . . . .
C25 C 0.22543(16) -0.22918(14) 0.71944(16) 0.0249 1.0000 Uani . . . . . .
C26 C 0.17601(18) -0.30341(15) 0.71404(18) 0.0316 1.0000 Uani . . . . . .
C27 C 0.14312(19) -0.29181(16) 0.6392(2) 0.0346 1.0000 Uani . . . . . .
C29 C 0.21295(16) -0.12968(14) 0.57258(16) 0.0241 1.0000 Uani . . . . . .
C30 C 0.24629(15) -0.13955(13) 0.64762(15) 0.0217 1.0000 Uani . . . . . .
C31 C 0.22120(16) -0.03911(14) 0.50550(16) 0.0245 1.0000 Uani . . . . . .
C32 C 0.26469(15) 0.12492(14) 0.43344(14) 0.0220 1.0000 Uani . . . . . .
C33 C 0.36297(16) 0.16284(14) 0.33342(14) 0.0231 1.0000 Uani . . . . . .
C34 C 0.46102(16) 0.13495(15) 0.34812(14) 0.0235 1.0000 Uani . . . . . .
C35 C 0.51121(15) 0.19702(13) 0.44739(14) 0.0216 1.0000 Uani . . . . . .
C36 C 0.52238(15) 0.20072(13) 0.53343(15) 0.0216 1.0000 Uani . . . . . .
C37 C 0.58607(18) 0.27704(16) 0.52239(18) 0.0307 1.0000 Uani . . . . . .
C38 C 0.6077(2) 0.27979(18) 0.5989(2) 0.0380 1.0000 Uani . . . . . .
C39 C 0.56843(19) 0.20537(17) 0.68822(18) 0.0328 1.0000 Uani . . . . . .
C40 C 0.50623(16) 0.12977(14) 0.70046(15) 0.0236 1.0000 Uani . . . . . .
C41 C 0.47917(15) 0.12602(13) 0.62355(14) 0.0203 1.0000 Uani . . . . . .
C42 C 0.5027(2) 0.05011(17) 0.85808(18) 0.0338 1.0000 Uani . . . . . .
C43 C 0.3677(2) 0.26882(16) 0.29715(18) 0.0347 1.0000 Uani . . . . . .
C44 C 0.3572(2) 0.1211(2) 0.25714(18) 0.0383 1.0000 Uani . . . . . .
C45 C -0.1251(2) 0.3529(2) 0.8686(2) 0.0448 1.0000 Uani . . . . . .
C46 C -0.1012(2) 0.2624(2) 0.9155(2) 0.0403 1.0000 Uani . . . . . .
C49 C 0.1795(3) -0.5629(2) 0.9830(3) 0.0610 1.0000 Uani . . . . . .
C50 C 0.1182(3) -0.5591(2) 0.9297(3) 0.0593 1.0000 Uani . . . . . .
C67 C 0.22551(19) 0.38298(15) 0.59325(17) 0.0312 1.0000 Uani . . . . . .
N1 N 0.54606(15) -0.63427(12) 1.00916(14) 0.0270 1.0000 Uani . . . . . .
N2 N 0.34264(15) -0.55452(13) 1.09734(15) 0.0293 1.0000 Uani . . . . . .
N3 N 0.47484(15) -0.49343(12) 0.87478(14) 0.0273 1.0000 Uani . . . . . .
N4 N 0.27522(14) 0.26792(12) 0.71449(14) 0.0257 1.0000 Uani . . . . . .
N5 N 0.11397(13) 0.22953(12) 0.68077(13) 0.0236 1.0000 Uani . . . . . .
N6 N 0.27551(13) 0.03403(11) 0.49416(12) 0.0206 1.0000 Uani . . . . . .
N7 N 0.45086(12) 0.13578(11) 0.44602(12) 0.0201 1.0000 Uani . . . . . .
N8 N -0.0823(2) 0.1917(2) 0.9515(2) 0.0532 1.0000 Uani . . . . . .
N10 N 0.0718(4) -0.5564(3) 0.8866(4) 0.1269 1.0000 Uani . . . . . .
O1 O 0.19990(13) 0.00125(11) 1.03642(12) 0.0285 1.0000 Uani . . . . . .
O2 O 0.20662(11) 0.10377(9) 0.86668(11) 0.0223 1.0000 Uani . . . . . .
O3 O 0.09835(11) 0.05324(10) 0.79778(10) 0.0223 1.0000 Uani . . . . . .
O4 O 0.02476(13) -0.12009(10) 0.85883(12) 0.0286 1.0000 Uani . . . . . .
O5 O 0.25921(13) -0.23255(10) 0.79059(12) 0.0303 1.0000 Uani . . . . . .
O6 O 0.29288(12) -0.07173(10) 0.65735(11) 0.0233 1.0000 Uani . . . . . .
O7 O 0.41844(12) 0.05317(10) 0.63950(11) 0.0232 1.0000 Uani . . . . . .
O8 O 0.46584(13) 0.05366(11) 0.78507(11) 0.0284 1.0000 Uani . . . . . .
K1 K 0.0000 0.0000 1.0000 0.0299 1.0000 Uani S . . . . .
K2 K 0.27207(5) -0.05943(3) 0.83071(4) 0.0341 1.0000 Uani . . . . . .
S1 S 0.62598(6) -0.80400(4) 1.00585(6) 0.0453 1.0000 Uani . . . . . .
S2 S 0.13808(7) -0.62739(9) 1.23927(8) 0.0866 1.0000 Uani . . . . . .
S3 S 0.44856(6) -0.46947(5) 0.70248(5) 0.0383 1.0000 Uani . . . . . .
C28 C 0.16122(18) -0.20616(15) 0.56946(19) 0.0312 1.0000 Uani . . . . . .
C47 C 0.6910(3) 0.3956(3) 0.7439(3) 0.0588(8) 1.0000 Uiso . . . . . .
C48 C 0.7712(4) 0.3453(3) 0.6918(3) 0.0676(11) 0.5000 Uiso . . . . . .
C480 C 0.7847(4) 0.3628(3) 0.6873(3) 0.0676(11) 0.5000 Uiso . . . . . .
N9 N 0.8313(5) 0.2997(5) 0.6523(4) 0.0976(18) 0.5000 Uiso . . . . . .
N90 N 0.8616(5) 0.3397(5) 0.6405(4) 0.0976(18) 0.5000 Uiso . . . . . .
H41 H 0.1702 -0.1176 1.1403 0.0483 1.0000 Uiso R . . . . .
H43 H 0.2786 -0.0627 1.1096 0.0469 1.0000 Uiso R . . . . .
H42 H 0.1715 -0.0317 1.1786 0.0467 1.0000 Uiso R . . . . .
H61 H 0.2898 0.0926 1.1086 0.0426 1.0000 Uiso R . . . . .
H71 H 0.3748 0.2442 1.0336 0.0508 1.0000 Uiso R . . . . .
H81 H 0.3920 0.3287 0.8770 0.0492 1.0000 Uiso R . . . . .
H111 H 0.3745 0.3385 0.7288 0.0367 1.0000 Uiso R . . . . .
H121 H 0.3248 0.2803 0.5701 0.0317 1.0000 Uiso R . . . . .
H122 H 0.3746 0.3635 0.5857 0.0323 1.0000 Uiso R . . . . .
H132 H 0.0673 0.3530 0.6386 0.0319 1.0000 Uiso R . . . . .
H131 H 0.0949 0.3397 0.7298 0.0324 1.0000 Uiso R . . . . .
H141 H 0.0332 0.2315 0.6084 0.0291 1.0000 Uiso R . . . . .
H161 H -0.0188 0.1061 0.5672 0.0379 1.0000 Uiso R . . . . .
H171 H -0.0724 -0.0506 0.6113 0.0430 1.0000 Uiso R . . . . .
H181 H -0.0550 -0.1576 0.7453 0.0379 1.0000 Uiso R . . . . .
H211 H 0.0078 -0.2473 0.8525 0.0475 1.0000 Uiso R . . . . .
H213 H -0.0190 -0.2412 0.9595 0.0482 1.0000 Uiso R . . . . .
H212 H -0.1006 -0.2117 0.9156 0.0476 1.0000 Uiso R . . . . .
H221 H 0.2959 0.5120 0.5666 0.0775 1.0000 Uiso R . . . . .
H223 H 0.1754 0.5072 0.6090 0.0774 1.0000 Uiso R . . . . .
H222 H 0.2239 0.4634 0.6819 0.0775 1.0000 Uiso R . . . . .
H231 H 0.1972 0.4444 0.4733 0.0606 1.0000 Uiso R . . . . .
H232 H 0.3177 0.4280 0.4401 0.0610 1.0000 Uiso R . . . . .
H233 H 0.2310 0.3429 0.4745 0.0612 1.0000 Uiso R . . . . .
H242 H 0.2828 -0.3157 0.9003 0.0552 1.0000 Uiso R . . . . .
H241 H 0.2856 -0.3655 0.8231 0.0549 1.0000 Uiso R . . . . .
H243 H 0.1743 -0.3455 0.9021 0.0545 1.0000 Uiso R . . . . .
H261 H 0.1644 -0.3618 0.7617 0.0353 1.0000 Uiso R . . . . .
H271 H 0.1086 -0.3427 0.6375 0.0425 1.0000 Uiso R . . . . .
H281 H 0.1380 -0.1978 0.5183 0.0400 1.0000 Uiso R . . . . .
H311 H 0.1807 -0.0319 0.4690 0.0304 1.0000 Uiso R . . . . .
H321 H 0.2545 0.1685 0.4722 0.0257 1.0000 Uiso R . . . . .
H322 H 0.2038 0.1199 0.4211 0.0250 1.0000 Uiso R . . . . .
H341 H 0.5226 0.1776 0.2946 0.0276 1.0000 Uiso R . . . . .
H342 H 0.4732 0.0720 0.3448 0.0277 1.0000 Uiso R . . . . .
H351 H 0.5539 0.2422 0.3856 0.0253 1.0000 Uiso R . . . . .
H371 H 0.6155 0.3256 0.4599 0.0368 1.0000 Uiso R . . . . .
H381 H 0.6509 0.3313 0.5919 0.0452 1.0000 Uiso R . . . . .
H391 H 0.5848 0.2074 0.7405 0.0416 1.0000 Uiso R . . . . .
H422 H 0.4787 0.1005 0.8868 0.0544 1.0000 Uiso R . . . . .
H421 H 0.4725 -0.0090 0.9104 0.0546 1.0000 Uiso R . . . . .
H423 H 0.5800 0.0527 0.8267 0.0543 1.0000 Uiso R . . . . .
H432 H 0.4227 0.2927 0.2306 0.0479 1.0000 Uiso R . . . . .
H431 H 0.3002 0.2854 0.3000 0.0477 1.0000 Uiso R . . . . .
H433 H 0.3814 0.2944 0.3415 0.0476 1.0000 Uiso R . . . . .
H442 H 0.4217 0.1381 0.1972 0.0603 1.0000 Uiso R . . . . .
H441 H 0.2989 0.1427 0.2434 0.0604 1.0000 Uiso R . . . . .
H443 H 0.3474 0.0540 0.2829 0.0602 1.0000 Uiso R . . . . .
H451 H -0.1961 0.3587 0.9079 0.0638 1.0000 Uiso R . . . . .
H452 H -0.1146 0.3560 0.8032 0.0643 1.0000 Uiso R . . . . .
H453 H -0.0797 0.4002 0.8663 0.0646 1.0000 Uiso R . . . . .
H491 H 0.2475 -0.5270 0.9386 0.0984 1.0000 Uiso R . . . . .
H493 H 0.1420 -0.5371 1.0372 0.0990 1.0000 Uiso R . . . . .
H492 H 0.1920 -0.6264 1.0081 0.0981 1.0000 Uiso R . . . . .
H474 H 0.7149 0.4579 0.7219 0.0703 0.5000 Uiso . . . . . .
H473 H 0.6315 0.3884 0.7335 0.0703 0.5000 Uiso . . . . . .
H475 H 0.6713 0.3713 0.8125 0.0703 0.5000 Uiso . . . . . .
H472 H 0.6330 0.3525 0.7640 0.0703 0.5000 Uiso . . . . . .
H471 H 0.6825 0.4524 0.7063 0.0703 0.5000 Uiso . . . . . .
H476 H 0.6929 0.4016 0.8008 0.0703 0.5000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.02245(11) 0.01638(10) 0.02554(11) -0.00412(8) -0.01335(9) 0.00096(8)
Ni1 0.01968(11) 0.01619(10) 0.02175(11) -0.00403(8) -0.00890(9) -0.00039(8)
Ni2 0.01869(11) 0.01650(10) 0.01890(10) -0.00291(8) -0.00924(9) -0.00018(8)
C1 0.0225(9) 0.0225(9) 0.0281(9) -0.0042(7) -0.0089(7) 0.0003(7)
C2 0.0280(11) 0.0424(14) 0.0419(13) -0.0007(11) -0.0180(10) 0.0024(10)
C3 0.0272(9) 0.0183(8) 0.0330(10) -0.0048(7) -0.0154(8) -0.0006(7)
C4 0.0338(11) 0.0332(11) 0.0281(10) -0.0102(8) -0.0185(9) 0.0069(9)
C5 0.0232(9) 0.0265(9) 0.0296(9) -0.0135(8) -0.0148(8) 0.0038(7)
C6 0.0305(10) 0.0378(12) 0.0361(11) -0.0183(10) -0.0199(9) 0.0038(9)
C7 0.0384(13) 0.0389(13) 0.0529(15) -0.0257(12) -0.0269(12) 0.0005(10)
C8 0.0366(12) 0.0306(11) 0.0540(15) -0.0176(11) -0.0237(11) -0.0054(9)
C9 0.0275(10) 0.0239(9) 0.0378(11) -0.0123(8) -0.0159(9) -0.0018(7)
C10 0.0210(8) 0.0216(8) 0.0290(9) -0.0117(7) -0.0124(7) 0.0016(7)
C11 0.0272(10) 0.0207(9) 0.0408(12) -0.0085(8) -0.0132(9) -0.0043(7)
C12 0.0256(10) 0.0229(9) 0.0305(10) -0.0015(8) -0.0053(8) -0.0026(7)
C13 0.0274(10) 0.0215(9) 0.0305(10) -0.0050(8) -0.0083(8) 0.0067(7)
C14 0.0210(8) 0.0284(10) 0.0229(9) -0.0024(7) -0.0095(7) 0.0035(7)
C15 0.0204(8) 0.0279(9) 0.0208(8) -0.0053(7) -0.0097(7) 0.0015(7)
C16 0.0260(10) 0.0419(12) 0.0252(9) -0.0084(9) -0.0154(8) 0.0033(9)
C17 0.0291(10) 0.0475(14) 0.0338(11) -0.0182(10) -0.0199(9) 0.0030(9)
C18 0.0270(10) 0.0316(10) 0.0356(11) -0.0162(9) -0.0170(9) 0.0019(8)
C19 0.0219(8) 0.0247(9) 0.0263(9) -0.0096(7) -0.0124(7) 0.0027(7)
C20 0.0188(8) 0.0238(8) 0.0198(8) -0.0067(7) -0.0085(6) 0.0007(6)
C21 0.0324(11) 0.0201(9) 0.0419(12) -0.0070(8) -0.0173(10) -0.0014(8)
C22 0.0548(18) 0.0234(11) 0.074(2) -0.0137(13) -0.0231(16) 0.0026(11)
C23 0.0443(15) 0.0453(15) 0.0310(12) 0.0053(11) -0.0092(11) 0.0043(12)
C24 0.0504(15) 0.0236(10) 0.0343(12) 0.0025(9) -0.0170(11) 0.0028(10)
C25 0.0230(9) 0.0184(8) 0.0272(9) -0.0048(7) -0.0070(7) 0.0005(7)
C26 0.0296(10) 0.0183(9) 0.0390(12) -0.0061(8) -0.0096(9) -0.0016(7)
C27 0.0324(11) 0.0228(10) 0.0495(14) -0.0143(9) -0.0167(10) -0.0011(8)
C29 0.0221(9) 0.0209(8) 0.0312(10) -0.0092(7) -0.0128(8) 0.0020(7)
C30 0.0187(8) 0.0186(8) 0.0250(9) -0.0058(7) -0.0079(7) 0.0007(6)
C31 0.0229(9) 0.0249(9) 0.0292(10) -0.0095(7) -0.0140(8) 0.0031(7)
C32 0.0217(8) 0.0226(8) 0.0222(8) -0.0051(7) -0.0115(7) 0.0043(7)
C33 0.0260(9) 0.0244(9) 0.0186(8) -0.0046(7) -0.0110(7) 0.0022(7)
C34 0.0216(8) 0.0279(9) 0.0191(8) -0.0069(7) -0.0074(7) 0.0032(7)
C35 0.0170(8) 0.0208(8) 0.0222(8) -0.0020(6) -0.0073(6) 0.0020(6)
C36 0.0188(8) 0.0201(8) 0.0252(9) -0.0047(7) -0.0106(7) 0.0008(6)
C37 0.0312(11) 0.0255(10) 0.0324(11) -0.0020(8) -0.0153(9) -0.0070(8)
C38 0.0418(13) 0.0326(11) 0.0399(13) -0.0047(10) -0.0214(11) -0.0133(10)
C39 0.0359(12) 0.0335(11) 0.0334(11) -0.0079(9) -0.0204(10) -0.0059(9)
C40 0.0234(9) 0.0235(9) 0.0260(9) -0.0071(7) -0.0130(7) 0.0019(7)
C41 0.0188(8) 0.0192(8) 0.0242(8) -0.0067(6) -0.0107(7) 0.0028(6)
C42 0.0429(13) 0.0355(12) 0.0290(11) -0.0078(9) -0.0226(10) 0.0013(10)
C43 0.0357(12) 0.0277(11) 0.0312(11) 0.0024(8) -0.0135(9) 0.0020(9)
C44 0.0383(13) 0.0546(16) 0.0263(11) -0.0178(11) -0.0146(10) 0.0023(11)
C45 0.0357(13) 0.0542(17) 0.0387(14) -0.0077(12) -0.0154(11) 0.0058(12)
C46 0.0360(13) 0.0531(16) 0.0406(13) -0.0216(12) -0.0203(11) 0.0055(11)
C49 0.066(2) 0.0361(15) 0.088(3) -0.0052(16) -0.050(2) 0.0005(14)
C50 0.067(2) 0.0437(17) 0.063(2) 0.0016(15) -0.0350(18) -0.0155(15)
C67 0.0326(11) 0.0189(9) 0.0310(10) -0.0016(8) -0.0080(9) 0.0016(8)
N1 0.0294(9) 0.0218(8) 0.0303(9) -0.0062(7) -0.0148(7) 0.0029(6)
N2 0.0261(8) 0.0276(9) 0.0333(9) -0.0040(7) -0.0156(7) 0.0004(7)
N3 0.0300(9) 0.0222(8) 0.0329(9) -0.0066(7) -0.0178(8) 0.0010(7)
N4 0.0224(8) 0.0190(7) 0.0304(9) -0.0045(6) -0.0088(7) -0.0011(6)
N5 0.0217(7) 0.0204(7) 0.0227(7) -0.0027(6) -0.0069(6) 0.0027(6)
N6 0.0191(7) 0.0208(7) 0.0211(7) -0.0050(6) -0.0093(6) 0.0017(6)
N7 0.0180(7) 0.0210(7) 0.0191(7) -0.0040(6) -0.0077(6) 0.0024(5)
N8 0.0606(17) 0.0510(15) 0.0705(18) -0.0271(14) -0.0441(15) 0.0123(13)
N10 0.153(4) 0.112(4) 0.135(4) 0.018(3) -0.112(4) -0.049(3)
O1 0.0355(8) 0.0260(7) 0.0297(7) -0.0063(6) -0.0207(7) -0.0010(6)
O2 0.0261(7) 0.0181(6) 0.0271(7) -0.0073(5) -0.0151(6) -0.0017(5)
O3 0.0274(7) 0.0197(6) 0.0221(6) -0.0041(5) -0.0142(6) -0.0030(5)
O4 0.0370(8) 0.0192(6) 0.0341(8) -0.0037(6) -0.0222(7) -0.0032(6)
O5 0.0374(8) 0.0205(7) 0.0276(7) -0.0003(6) -0.0139(7) -0.0009(6)
O6 0.0274(7) 0.0181(6) 0.0228(6) -0.0022(5) -0.0118(6) -0.0039(5)
O7 0.0276(7) 0.0184(6) 0.0242(7) -0.0018(5) -0.0147(6) -0.0030(5)
O8 0.0348(8) 0.0270(7) 0.0260(7) -0.0032(6) -0.0188(6) -0.0022(6)
K1 0.0259(3) 0.0364(3) 0.0227(3) -0.0072(2) -0.0074(2) -0.0016(2)
K2 0.0432(3) 0.0257(2) 0.0307(2) -0.00794(18) -0.0145(2) 0.00483(19)
S1 0.0363(3) 0.0237(3) 0.0632(4) -0.0110(3) -0.0125(3) 0.0106(2)
S2 0.0254(3) 0.1166(9) 0.0716(6) 0.0159(6) -0.0078(4) -0.0087(5)
S3 0.0514(4) 0.0359(3) 0.0346(3) -0.0055(2) -0.0280(3) -0.0041(3)
C28 0.0313 0.0246 0.0451 -0.0149 -0.0208 0.0020
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 . N3 2_647 2.1053(19) yes
Mo1 . N2 2_647 2.0996(19) yes
Mo1 . N1 2_647 2.0982(18) yes
Mo1 . N1 . 2.0982(18) yes
Mo1 . N2 . 2.0996(19) yes
Mo1 . N3 . 2.1053(19) yes
Ni1 . N4 . 1.8694(17) yes
Ni1 . N5 . 1.8658(17) yes
Ni1 . O2 . 1.8550(14) yes
Ni1 . O3 . 1.8484(14) yes
Ni2 . N6 . 1.8655(16) yes
Ni2 . N7 . 1.8712(16) yes
Ni2 . O6 . 1.8526(14) yes
Ni2 . O7 . 1.8578(14) yes
C1 . N1 . 1.158(3) yes
C1 . S1 . 1.623(2) yes
C2 . N2 . 1.158(3) yes
C2 . S2 . 1.623(3) yes
C3 . N3 . 1.164(3) yes
C3 . S3 . 1.624(2) yes
C4 . O1 . 1.431(3) yes
C4 . H41 . 0.957 no
C4 . H43 . 0.972 no
C4 . H42 . 0.965 no
C5 . C6 . 1.379(3) yes
C5 . C10 . 1.420(3) yes
C5 . O1 . 1.372(3) yes
C6 . C7 . 1.403(3) yes
C6 . H61 . 0.941 no
C7 . C8 . 1.360(4) yes
C7 . H71 . 0.943 no
C8 . C9 . 1.415(3) yes
C8 . H81 . 0.941 no
C9 . C10 . 1.409(3) yes
C9 . C11 . 1.432(3) yes
C10 . O2 . 1.318(2) yes
C11 . N4 . 1.292(3) yes
C11 . H111 . 0.942 no
C12 . C67 . 1.532(3) yes
C12 . N4 . 1.472(3) yes
C12 . H121 . 0.981 no
C12 . H122 . 0.977 no
C13 . C67 . 1.531(3) yes
C13 . N5 . 1.472(3) yes
C13 . H132 . 0.954 no
C13 . H131 . 0.974 no
C14 . C15 . 1.436(3) yes
C14 . N5 . 1.290(3) yes
C14 . H141 . 0.940 no
C15 . C16 . 1.411(3) yes
C15 . C20 . 1.411(3) yes
C16 . C17 . 1.366(3) yes
C16 . H161 . 0.946 no
C17 . C18 . 1.406(3) yes
C17 . H171 . 0.948 no
C18 . C19 . 1.376(3) yes
C18 . H181 . 0.939 no
C19 . C20 . 1.426(3) yes
C19 . O4 . 1.367(2) yes
C20 . O3 . 1.312(2) yes
C21 . O4 . 1.432(2) yes
C21 . H211 . 0.968 no
C21 . H213 . 0.949 no
C21 . H212 . 0.979 no
C22 . C67 . 1.531(4) yes
C22 . H221 . 0.947 no
C22 . H223 . 0.945 no
C22 . H222 . 0.973 no
C23 . C67 . 1.532(4) yes
C23 . H231 . 0.950 no
C23 . H232 . 0.986 no
C23 . H233 . 0.982 no
C24 . O5 . 1.428(3) yes
C24 . H242 . 0.968 no
C24 . H241 . 0.980 no
C24 . H243 . 0.986 no
C25 . C26 . 1.380(3) yes
C25 . C30 . 1.425(3) yes
C25 . O5 . 1.373(3) yes
C26 . C27 . 1.398(4) yes
C26 . H261 . 0.937 no
C27 . C28 . 1.372(3) yes
C27 . H271 . 0.937 no
C29 . C30 . 1.409(3) yes
C29 . C31 . 1.432(3) yes
C29 . C28 . 1.409(3) yes
C30 . O6 . 1.313(2) yes
C31 . N6 . 1.289(3) yes
C31 . H311 . 0.952 no
C32 . C33 . 1.533(3) yes
C32 . N6 . 1.471(2) yes
C32 . H321 . 0.985 no
C32 . H322 . 0.971 no
C33 . C34 . 1.531(3) yes
C33 . C43 . 1.528(3) yes
C33 . C44 . 1.531(3) yes
C34 . N7 . 1.474(3) yes
C34 . H341 . 0.981 no
C34 . H342 . 0.974 no
C35 . C36 . 1.433(3) yes
C35 . N7 . 1.288(2) yes
C35 . H351 . 0.948 no
C36 . C37 . 1.408(3) yes
C36 . C41 . 1.413(3) yes
C37 . C38 . 1.365(3) yes
C37 . H371 . 0.954 no
C38 . C39 . 1.403(3) yes
C38 . H381 . 0.954 no
C39 . C40 . 1.379(3) yes
C39 . H391 . 0.946 no
C40 . C41 . 1.423(3) yes
C40 . O8 . 1.376(2) yes
C41 . O7 . 1.313(2) yes
C42 . O8 . 1.431(3) yes
C42 . H422 . 0.974 no
C42 . H421 . 0.971 no
C42 . H423 . 0.984 no
C43 . H432 . 0.956 no
C43 . H431 . 0.968 no
C43 . H433 . 0.971 no
C44 . H442 . 0.954 no
C44 . H441 . 0.965 no
C44 . H443 . 0.965 no
C45 . C46 . 1.458(4) yes
C45 . H451 . 0.944 no
C45 . H452 . 0.951 no
C45 . H453 . 0.958 no
C46 . N8 . 1.137(4) yes
C49 . C50 . 1.428(5) yes
C49 . H491 . 0.968 no
C49 . H493 . 0.970 no
C49 . H492 . 0.968 no
C50 . N10 . 1.118(5) yes
C28 . H281 . 0.962 no
C47 . C48 . 1.430(6) yes
C47 . C480 . 1.413(6) yes
C47 . H474 . 0.921 no
C47 . H473 . 0.939 no
C47 . H475 . 0.935 no
C47 . H472 . 0.942 no
C47 . H471 . 0.926 no
C47 . H476 . 0.929 no
C48 . N9 . 1.158(6) yes
C480 . N90 . 1.132(6) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 2_647 Mo1 . N2 2_647 91.20(7) yes
N3 2_647 Mo1 . N1 2_647 91.36(7) yes
N2 2_647 Mo1 . N1 2_647 91.24(7) yes
N3 2_647 Mo1 . N1 . 88.64(7) yes
N2 2_647 Mo1 . N1 . 88.76(7) yes
N1 2_647 Mo1 . N1 . 179.995 yes
N3 2_647 Mo1 . N2 . 88.80(7) yes
N2 2_647 Mo1 . N2 . 179.995 yes
N1 2_647 Mo1 . N2 . 88.76(7) yes
N1 . Mo1 . N2 . 91.24(7) yes
N3 2_647 Mo1 . N3 . 179.995 yes
N2 2_647 Mo1 . N3 . 88.80(7) yes
N1 2_647 Mo1 . N3 . 88.64(7) yes
N1 . Mo1 . N3 . 91.36(7) yes
N2 . Mo1 . N3 . 91.20(7) yes
N4 . Ni1 . N5 . 91.17(8) yes
N4 . Ni1 . O2 . 94.24(7) yes
N5 . Ni1 . O2 . 167.07(7) yes
N4 . Ni1 . O3 . 168.71(7) yes
N5 . Ni1 . O3 . 93.61(7) yes
O2 . Ni1 . O3 . 83.26(6) yes
N6 . Ni2 . N7 . 90.41(7) yes
N6 . Ni2 . O6 . 92.70(7) yes
N7 . Ni2 . O6 . 168.12(7) yes
N6 . Ni2 . O7 . 167.03(7) yes
N7 . Ni2 . O7 . 94.62(7) yes
O6 . Ni2 . O7 . 84.80(6) yes
N1 . C1 . S1 . 178.0(2) yes
N2 . C2 . S2 . 179.7(2) yes
N3 . C3 . S3 . 179.0(2) yes
O1 . C4 . H41 . 107.6 no
O1 . C4 . H43 . 108.5 no
H41 . C4 . H43 . 109.5 no
O1 . C4 . H42 . 110.0 no
H41 . C4 . H42 . 110.9 no
H43 . C4 . H42 . 110.4 no
C6 . C5 . C10 . 121.1(2) yes
C6 . C5 . O1 . 124.5(2) yes
C10 . C5 . O1 . 114.41(17) yes
C5 . C6 . C7 . 120.2(2) yes
C5 . C6 . H61 . 120.5 no
C7 . C6 . H61 . 119.2 no
C6 . C7 . C8 . 119.9(2) yes
C6 . C7 . H71 . 120.1 no
C8 . C7 . H71 . 120.0 no
C7 . C8 . C9 . 121.0(2) yes
C7 . C8 . H81 . 120.6 no
C9 . C8 . H81 . 118.4 no
C8 . C9 . C10 . 119.9(2) yes
C8 . C9 . C11 . 119.2(2) yes
C10 . C9 . C11 . 120.68(19) yes
C5 . C10 . C9 . 117.68(18) yes
C5 . C10 . O2 . 118.17(17) yes
C9 . C10 . O2 . 124.14(19) yes
C9 . C11 . N4 . 125.66(19) yes
C9 . C11 . H111 . 117.3 no
N4 . C11 . H111 . 117.0 no
C67 . C12 . N4 . 112.75(18) yes
C67 . C12 . H121 . 108.9 no
N4 . C12 . H121 . 107.3 no
C67 . C12 . H122 . 110.1 no
N4 . C12 . H122 . 109.6 no
H121 . C12 . H122 . 108.1 no
C67 . C13 . N5 . 112.59(17) yes
C67 . C13 . H132 . 109.5 no
N5 . C13 . H132 . 107.9 no
C67 . C13 . H131 . 108.6 no
N5 . C13 . H131 . 107.3 no
H132 . C13 . H131 . 111.0 no
C15 . C14 . N5 . 125.38(19) yes
C15 . C14 . H141 . 116.9 no
N5 . C14 . H141 . 117.7 no
C14 . C15 . C16 . 119.28(19) yes
C14 . C15 . C20 . 119.93(18) yes
C16 . C15 . C20 . 120.33(19) yes
C15 . C16 . C17 . 120.2(2) yes
C15 . C16 . H161 . 119.0 no
C17 . C16 . H161 . 120.7 no
C16 . C17 . C18 . 120.5(2) yes
C16 . C17 . H171 . 119.5 no
C18 . C17 . H171 . 120.0 no
C17 . C18 . C19 . 120.2(2) yes
C17 . C18 . H181 . 119.6 no
C19 . C18 . H181 . 120.2 no
C18 . C19 . C20 . 120.73(19) yes
C18 . C19 . O4 . 125.50(19) yes
C20 . C19 . O4 . 113.77(17) yes
C19 . C20 . C15 . 117.86(17) yes
C19 . C20 . O3 . 117.68(17) yes
C15 . C20 . O3 . 124.37(18) yes
O4 . C21 . H211 . 109.7 no
O4 . C21 . H213 . 107.1 no
H211 . C21 . H213 . 110.4 no
O4 . C21 . H212 . 109.0 no
H211 . C21 . H212 . 111.1 no
H213 . C21 . H212 . 109.5 no
C67 . C22 . H221 . 110.4 no
C67 . C22 . H223 . 108.0 no
H221 . C22 . H223 . 108.8 no
C67 . C22 . H222 . 110.5 no
H221 . C22 . H222 . 110.9 no
H223 . C22 . H222 . 108.1 no
C67 . C23 . H231 . 107.7 no
C67 . C23 . H232 . 108.7 no
H231 . C23 . H232 . 110.5 no
C67 . C23 . H233 . 109.8 no
H231 . C23 . H233 . 111.0 no
H232 . C23 . H233 . 109.1 no
O5 . C24 . H242 . 108.0 no
O5 . C24 . H241 . 110.1 no
H242 . C24 . H241 . 108.5 no
O5 . C24 . H243 . 109.8 no
H242 . C24 . H243 . 109.9 no
H241 . C24 . H243 . 110.5 no
C26 . C25 . C30 . 120.8(2) yes
C26 . C25 . O5 . 125.42(19) yes
C30 . C25 . O5 . 113.74(17) yes
C25 . C26 . C27 . 120.7(2) yes
C25 . C26 . H261 . 118.9 no
C27 . C26 . H261 . 120.4 no
C26 . C27 . C28 . 119.8(2) yes
C26 . C27 . H271 . 119.4 no
C28 . C27 . H271 . 120.7 no
C30 . C29 . C31 . 119.63(18) yes
C30 . C29 . C28 . 120.70(19) yes
C31 . C29 . C28 . 119.3(2) yes
C25 . C30 . C29 . 117.44(18) yes
C25 . C30 . O6 . 117.84(18) yes
C29 . C30 . O6 . 124.70(18) yes
C29 . C31 . N6 . 124.98(19) yes
C29 . C31 . H311 . 117.3 no
N6 . C31 . H311 . 117.6 no
C33 . C32 . N6 . 112.27(16) yes
C33 . C32 . H321 . 108.5 no
N6 . C32 . H321 . 107.1 no
C33 . C32 . H322 . 109.4 no
N6 . C32 . H322 . 109.9 no
H321 . C32 . H322 . 109.5 no
C32 . C33 . C34 . 109.25(15) yes
C32 . C33 . C43 . 108.68(17) yes
C34 . C33 . C43 . 110.16(18) yes
C32 . C33 . C44 . 109.46(18) yes
C34 . C33 . C44 . 108.90(18) yes
C43 . C33 . C44 . 110.37(19) yes
C33 . C34 . N7 . 112.40(16) yes
C33 . C34 . H341 . 109.3 no
N7 . C34 . H341 . 109.6 no
C33 . C34 . H342 . 110.3 no
N7 . C34 . H342 . 106.9 no
H341 . C34 . H342 . 108.3 no
C36 . C35 . N7 . 125.74(17) yes
C36 . C35 . H351 . 117.1 no
N7 . C35 . H351 . 117.1 no
C35 . C36 . C37 . 117.77(18) yes
C35 . C36 . C41 . 120.98(17) yes
C37 . C36 . C41 . 120.99(19) yes
C36 . C37 . C38 . 120.3(2) yes
C36 . C37 . H371 . 118.8 no
C38 . C37 . H371 . 120.9 no
C37 . C38 . C39 . 120.0(2) yes
C37 . C38 . H381 . 120.7 no
C39 . C38 . H381 . 119.3 no
C38 . C39 . C40 . 120.7(2) yes
C38 . C39 . H391 . 119.4 no
C40 . C39 . H391 . 119.9 no
C39 . C40 . C41 . 120.86(19) yes
C39 . C40 . O8 . 124.18(19) yes
C41 . C40 . O8 . 114.96(17) yes
C40 . C41 . C36 . 117.15(17) yes
C40 . C41 . O7 . 118.49(17) yes
C36 . C41 . O7 . 124.34(18) yes
O8 . C42 . H422 . 110.2 no
O8 . C42 . H421 . 106.9 no
H422 . C42 . H421 . 108.9 no
O8 . C42 . H423 . 109.1 no
H422 . C42 . H423 . 112.0 no
H421 . C42 . H423 . 109.5 no
C33 . C43 . H432 . 109.6 no
C33 . C43 . H431 . 109.1 no
H432 . C43 . H431 . 111.2 no
C33 . C43 . H433 . 109.0 no
H432 . C43 . H433 . 109.8 no
H431 . C43 . H433 . 108.1 no
C33 . C44 . H442 . 110.2 no
C33 . C44 . H441 . 109.2 no
H442 . C44 . H441 . 110.6 no
C33 . C44 . H443 . 110.3 no
H442 . C44 . H443 . 107.1 no
H441 . C44 . H443 . 109.4 no
C46 . C45 . H451 . 108.1 no
C46 . C45 . H452 . 109.0 no
H451 . C45 . H452 . 110.0 no
C46 . C45 . H453 . 108.4 no
H451 . C45 . H453 . 110.2 no
H452 . C45 . H453 . 111.1 no
C45 . C46 . N8 . 179.6(3) yes
C50 . C49 . H491 . 109.9 no
C50 . C49 . H493 . 108.2 no
H491 . C49 . H493 . 109.9 no
C50 . C49 . H492 . 110.3 no
H491 . C49 . H492 . 107.3 no
H493 . C49 . H492 . 111.1 no
C49 . C50 . N10 . 178.7(6) yes
C12 . C67 . C23 . 108.3(2) yes
C12 . C67 . C22 . 110.5(2) yes
C23 . C67 . C22 . 110.3(2) yes
C12 . C67 . C13 . 109.57(17) yes
C23 . C67 . C13 . 109.9(2) yes
C22 . C67 . C13 . 108.3(2) yes
Mo1 . N1 . C1 . 175.22(18) yes
Mo1 . N2 . C2 . 175.1(2) yes
Mo1 . N3 . C3 . 174.78(17) yes
C12 . N4 . C11 . 118.75(18) yes
C12 . N4 . Ni1 . 115.66(15) yes
C11 . N4 . Ni1 . 125.21(15) yes
C13 . N5 . C14 . 118.76(18) yes
C13 . N5 . Ni1 . 115.04(15) yes
C14 . N5 . Ni1 . 125.76(15) yes
C32 . N6 . C31 . 118.87(17) yes
C32 . N6 . Ni2 . 114.76(12) yes
C31 . N6 . Ni2 . 126.14(14) yes
C34 . N7 . C35 . 117.96(16) yes
C34 . N7 . Ni2 . 116.29(13) yes
C35 . N7 . Ni2 . 125.42(14) yes
C4 . O1 . C5 . 116.21(16) yes
C10 . O2 . Ni1 . 125.50(13) yes
C20 . O3 . Ni1 . 126.09(12) yes
C21 . O4 . C19 . 116.08(17) yes
C24 . O5 . C25 . 116.52(18) yes
C30 . O6 . Ni2 . 124.93(13) yes
C41 . O7 . Ni2 . 126.17(12) yes
C42 . O8 . C40 . 115.99(17) yes
C29 . C28 . C27 . 120.5(2) yes
C29 . C28 . H281 . 119.5 no
C27 . C28 . H281 . 120.0 no
C48 . C47 . H474 . 110.5 no
C480 . C47 . H474 . 98.9 no
C48 . C47 . H473 . 109.6 no
C480 . C47 . H473 . 118.5 no
H474 . C47 . H473 . 109.5 no
C48 . C47 . H475 . 109.2 no
C480 . C47 . H475 . 111.4 no
H474 . C47 . H475 . 109.8 no
H473 . C47 . H475 . 108.2 no
C48 . C47 . H472 . 97.2 no
C480 . C47 . H472 . 109.4 no
H474 . C47 . H472 . 144.8 no
H475 . C47 . H472 . 79.3 no
C48 . C47 . H471 . 117.0 no
C480 . C47 . H471 . 110.6 no
H473 . C47 . H471 . 71.0 no
H475 . C47 . H471 . 131.2 no
C48 . C47 . H476 . 114.4 no
C480 . C47 . H476 . 109.7 no
H474 . C47 . H476 . 79.9 no
H473 . C47 . H476 . 127.9 no
H472 . C47 . H471 . 108.8 no
H472 . C47 . H476 . 108.5 no
H471 . C47 . H476 . 109.9 no
C47 . C48 . N9 . 175.6(6) yes
C47 . C480 . N90 . 177.5(6) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C34 . H342 . O7 2_656 145 0.97 2.43 3.276(4) yes
C45 . H453 . N10 1_565 149 0.96 2.43 3.294(4) yes
# Hand-made tables can be put in the cif. The number of columns
# is set in the loop header.
# The contants of each column can either be a piece of text
# without any spaces (eg a number) or other text enclosed in " "
# Remove the leading # in the following example
#geom_extra_table_head_A
#;
#Table 2.
#Molecular parameters deviating most from MOGUL averages
#;
#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
#_geom_extra_tableA_col_4
#
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d"
#N5-C6-C4 129 124 "7 (\%)"
#C3-O10-C2 105 109 "2 (\%)"
#C6-O7 1.25 1.22 ".02 (\%A)"
#
data_1
_database_code_depnum_ccdc_archive 'CCDC 809268'
#TrackingRef '- Compd_2new.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 23.3664(8)
_cell_length_b 37.452(2)
_cell_length_c 12.1573(8)
_cell_angle_alpha 90
_cell_angle_beta 105.626(6)
_cell_angle_gamma 90
_cell_volume 10246.0(10)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 1 2/m 1 '
_symmetry_space_group_name_Hall '-C 2y'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z
x,-y,z
-x+1/2,y+1/2,-z
x+1/2,-y+1/2,z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C85 H108 K2 Mo1 N17 Ni3 O14 S6
# Dc = 1.38 Fooo = 4420.00 Mu = 9.31 M = 1067.28
# Found Formula = C85 H104 K2 Mo1 N17 Ni3 O14 S6
# Dc = 1.38 FOOO = 4420.00 Mu = 9.30 M = 1065.26
_chemical_formula_sum 'C85 H108 K2 Mo1 N17 Ni3 O14 S6'
_chemical_formula_moiety
;
3(C21 H24 N2 Ni1 O4),K2,(C8 H20 N),(C6 Mo N6 S6),4(C2 H3 N), 2(H2 O)
;
_chemical_compound_source ?
_chemical_formula_weight 2134.56
_cell_measurement_reflns_used 9586
_cell_measurement_theta_min 3
_cell_measurement_theta_max 29
_cell_measurement_temperature 180
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.150
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_max 0.250
_exptl_crystal_density_diffrn 1.384
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 4420
_exptl_absorpt_coefficient_mu 0.931
# Sheldrick geometric approximatio 0.87 0.87
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min 0.82
_exptl_absorpt_correction_T_max 0.87
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 180
_diffrn_reflns_number 48950
_reflns_number_total 14120
_diffrn_reflns_av_R_equivalents 0.075
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 14120
# Theoretical number of reflections is about 27965
_diffrn_reflns_theta_min 2.829
_diffrn_reflns_theta_max 29.301
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 28.715
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_k_min -51
_diffrn_reflns_limit_k_max 51
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_reflns_limit_h_min -32
_reflns_limit_h_max 30
_reflns_limit_k_min 0
_reflns_limit_k_max 51
_reflns_limit_l_min 0
_reflns_limit_l_max 16
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.84
_refine_diff_density_max 1.80
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>1.8\s(I)
_refine_ls_number_reflns 5855
_refine_ls_number_restraints 12
_refine_ls_number_parameters 582
_oxford_refine_ls_R_factor_ref 0.0639
_refine_ls_wR_factor_ref 0.0653
_refine_ls_goodness_of_fit_ref 1.0872
_refine_ls_shift/su_max 0.0099963
_refine_ls_shift/su_mean 0.0000640
# The values computed from all data
_oxford_reflns_number_all 14088
_refine_ls_R_factor_all 0.1509
_refine_ls_wR_factor_all 0.1563
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 5635
_refine_ls_R_factor_gt 0.0620
_refine_ls_wR_factor_gt 0.0641
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.436 0.460 0.192
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Mo1 Mo 0.75302(5) 0.5000 0.28524(9) 0.0627 1.0000 Uani S T . . . .
Ni1 Ni 0.68658(3) 0.754434(19) 0.07457(6) 0.0296 1.0000 Uani . . . . . .
Ni2 Ni 0.5000 0.77089(3) 0.0000 0.0302 1.0000 Uani S T . . . .
K1 K 0.57411(5) 0.68621(3) -0.03747(10) 0.0368 1.0000 Uani . . . . . .
C1 C 0.8144(3) 0.55884(18) 0.1609(6) 0.0554 1.0000 Uani . . . . . .
C2 C 0.8726(10) 0.5000 0.4787(18) 0.1062 1.0000 Uani S T . . . .
C3 C 0.6931(4) 0.55773(19) 0.4153(7) 0.0670 1.0000 Uani . . . . . .
C4 C 0.6454(6) 0.5000 0.0547(14) 0.0724 1.0000 Uani S T . . . .
C5 C 0.6682(4) 0.60089(18) 0.0782(7) 0.0645 1.0000 Uani . . . . . .
C6 C 0.7055(3) 0.65193(17) 0.1876(5) 0.0382 1.0000 Uani . . . . . .
C7 C 0.7363(3) 0.63233(19) 0.2776(6) 0.0485 1.0000 Uani . . . . . .
C8 C 0.7677(3) 0.6485(2) 0.3792(6) 0.0540 1.0000 Uani . . . . . .
C9 C 0.7679(3) 0.6844(2) 0.3865(5) 0.0461 1.0000 Uani . . . . . .
C10 C 0.7380(2) 0.70544(17) 0.2946(4) 0.0351 1.0000 Uani . . . . . .
C11 C 0.7064(2) 0.68965(16) 0.1917(4) 0.0327 1.0000 Uani . . . . . .
C12 C 0.7343(2) 0.74293(17) 0.3075(5) 0.0348 1.0000 Uani . . . . . .
C13 C 0.7063(3) 0.80191(16) 0.2586(5) 0.0380 1.0000 Uani . . . . . .
C14 C 0.7487(2) 0.82755(16) 0.2237(5) 0.0371 1.0000 Uani . . . . . .
C15 C 0.7601(2) 0.81543(16) 0.1132(5) 0.0365 1.0000 Uani . . . . . .
C16 C 0.6863(2) 0.81419(15) -0.0619(5) 0.0355 1.0000 Uani . . . . . .
C17 C 0.6421(2) 0.80014(16) -0.1558(4) 0.0330 1.0000 Uani . . . . . .
C18 C 0.6203(3) 0.82128(18) -0.2512(5) 0.0429 1.0000 Uani . . . . . .
C19 C 0.5816(3) 0.80792(19) -0.3462(5) 0.0493 1.0000 Uani . . . . . .
C20 C 0.5651(3) 0.7728(2) -0.3486(5) 0.0458 1.0000 Uani . . . . . .
C21 C 0.5865(2) 0.75095(17) -0.2568(4) 0.0339 1.0000 Uani . . . . . .
C22 C 0.6252(2) 0.76423(15) -0.1554(4) 0.0283 1.0000 Uani . . . . . .
C23 C 0.5426(3) 0.6997(2) -0.3562(5) 0.0488 1.0000 Uani . . . . . .
C24 C 0.8075(3) 0.82740(19) 0.3149(6) 0.0508 1.0000 Uani . . . . . .
C25 C 0.7216(3) 0.86442(18) 0.2122(6) 0.0526 1.0000 Uani . . . . . .
C26 C 0.4194(3) 0.6444(2) -0.2711(6) 0.0641 1.0000 Uani . . . . . .
C27 C 0.4210(2) 0.70743(19) -0.2680(5) 0.0401 1.0000 Uani . . . . . .
C28 C 0.3863(3) 0.7097(2) -0.3780(5) 0.0463 1.0000 Uani . . . . . .
C29 C 0.3773(3) 0.7426(2) -0.4339(5) 0.0515 1.0000 Uani . . . . . .
C30 C 0.4025(3) 0.7721(2) -0.3798(5) 0.0455 1.0000 Uani . . . . . .
C31 C 0.4365(2) 0.77021(17) -0.2664(5) 0.0356 1.0000 Uani . . . . . .
C32 C 0.4456(2) 0.73835(16) -0.2077(4) 0.0320 1.0000 Uani . . . . . .
C33 C 0.4659(2) 0.80165(18) -0.2159(5) 0.0403 1.0000 Uani . . . . . .
C34 C 0.5268(3) 0.83826(16) -0.0741(5) 0.0396 1.0000 Uani . . . . . .
C35 C 0.5000 0.8618(2) 0.0000 0.0405 1.0000 Uani S T . . . .
C36 C 0.5486(3) 0.8844(2) 0.0752(7) 0.0655 1.0000 Uani . . . . . .
C37 C 0.9104(7) 0.5883(4) 0.4282(12) 0.1526 1.0000 Uani . . . . . .
C38 C 0.9181(6) 0.6101(3) 0.5255(10) 0.1070 1.0000 Uani . . . . . .
C39 C 0.5564(8) 0.5703(4) -0.3226(13) 0.1758 1.0000 Uani . . . . . .
C40 C 0.5709(5) 0.6006(3) -0.2500(9) 0.0863 1.0000 Uani . . . . . .
N1 N 0.7915(3) 0.53881(14) 0.2070(5) 0.0585 1.0000 Uani . . . . . .
N2 N 0.8264(6) 0.5000 0.4178(12) 0.0824 1.0000 Uani S T . . . .
N3 N 0.7149(3) 0.53854(16) 0.3657(6) 0.0737 1.0000 Uani . . . . . .
N4 N 0.6795(5) 0.5000 0.1408(11) 0.0717 1.0000 Uani S T . . . .
N5 N 0.71487(19) 0.76519(12) 0.2280(4) 0.0317 1.0000 Uani . . . . . .
N6 N 0.70806(19) 0.79910(13) 0.0340(4) 0.0329 1.0000 Uani . . . . . .
N7 N 0.4931(2) 0.80573(12) -0.1104(4) 0.0336 1.0000 Uani . . . . . .
N8 N 0.9265(7) 0.6283(3) 0.5965(9) 0.1590 1.0000 Uani . . . . . .
N9 N 0.5798(4) 0.6233(2) -0.1936(7) 0.0895 1.0000 Uani . . . . . .
O1 O 0.67129(18) 0.63855(11) 0.0881(3) 0.0423 1.0000 Uani . . . . . .
O2 O 0.67633(16) 0.70714(10) 0.1033(3) 0.0337 1.0000 Uani . . . . . .
O3 O 0.64390(16) 0.74276(10) -0.0699(3) 0.0327 1.0000 Uani . . . . . .
O4 O 0.57360(17) 0.71566(11) -0.2519(3) 0.0388 1.0000 Uani . . . . . .
O5 O 0.43545(19) 0.67648(12) -0.2081(3) 0.0460 1.0000 Uani . . . . . .
O6 O 0.47730(16) 0.73424(10) -0.1026(3) 0.0338 1.0000 Uani . . . . . .
S1 S 0.84615(13) 0.58691(6) 0.0977(2) 0.0872 1.0000 Uani . . . . . .
S2 S 0.9393(3) 0.5000 0.5680(6) 0.1808 1.0000 Uani S T . . . .
S3 S 0.66442(15) 0.58476(6) 0.4888(2) 0.1040 1.0000 Uani . . . . . .
S4 S 0.5952(2) 0.5000 -0.0669(5) 0.1218 1.0000 Uani S T . . . .
C41 C 0.8378(13) 0.520594(10) 0.827(3) 0.158(11) 0.5000 Uiso D . . . . .
C42 C 0.8488(15) 0.5464(9) 0.752(3) 0.162(13) 0.5000 Uiso D . . . . .
C43 C 0.7834(11) 0.479726(10) 0.683(2) 0.125(8) 0.5000 Uiso D . . . . .
C44 C 0.8275(11) 0.4495(6) 0.682(2) 0.110(8) 0.5000 Uiso D . . . . .
C45 C 0.7257(14) 0.518242(10) 0.725(3) 0.182(14) 0.5000 Uiso D . . . . .
C46 C 0.7063(18) 0.5458(10) 0.809(3) 0.188(16) 0.5000 Uiso D . . . . .
C47 C 0.7746(12) 0.484614(10) 0.890(2) 0.155(11) 0.5000 Uiso D . . . . .
C48 C 0.7305(9) 0.4562(6) 0.871(2) 0.089(6) 0.5000 Uiso D . . . . .
N10 N 0.7827(4) 0.5000 0.7832(8) 0.069(2) 1.0000 Uiso DS . . . . .
O7 O 0.5000 0.6235(3) 0.0000 0.108(3) 1.0000 Uiso S . . . . .
O8 O 1.0590(13) 0.5000 0.813(2) 0.162(10) 0.5000 Uiso S . . . . .
O9 O 0.4317(15) 0.5000 0.667(3) 0.182(12) 0.5000 Uiso S . . . . .
H51 H 0.6448 0.5947 0.0026 0.0988 1.0000 Uiso R . . . . .
H53 H 0.7078 0.5915 0.0910 0.0989 1.0000 Uiso R . . . . .
H52 H 0.6505 0.5915 0.1347 0.0991 1.0000 Uiso R . . . . .
H71 H 0.7360 0.6076 0.2716 0.0601 1.0000 Uiso R . . . . .
H81 H 0.7885 0.6346 0.4402 0.0651 1.0000 Uiso R . . . . .
H91 H 0.7885 0.6956 0.4546 0.0581 1.0000 Uiso R . . . . .
H121 H 0.7477 0.7519 0.3818 0.0402 1.0000 Uiso R . . . . .
H131 H 0.7114 0.8035 0.3409 0.0469 1.0000 Uiso R . . . . .
H132 H 0.6660 0.8088 0.2183 0.0470 1.0000 Uiso R . . . . .
H151 H 0.7722 0.8360 0.0768 0.0450 1.0000 Uiso R . . . . .
H152 H 0.7922 0.7981 0.1304 0.0451 1.0000 Uiso R . . . . .
H161 H 0.7007 0.8371 -0.0714 0.0413 1.0000 Uiso R . . . . .
H181 H 0.6329 0.8450 -0.2492 0.0542 1.0000 Uiso R . . . . .
H191 H 0.5659 0.8226 -0.4091 0.0591 1.0000 Uiso R . . . . .
H201 H 0.5392 0.7631 -0.4142 0.0561 1.0000 Uiso R . . . . .
H231 H 0.5366 0.6748 -0.3422 0.0721 1.0000 Uiso R . . . . .
H232 H 0.5649 0.7022 -0.4122 0.0719 1.0000 Uiso R . . . . .
H233 H 0.5045 0.7114 -0.3845 0.0719 1.0000 Uiso R . . . . .
H242 H 0.8357 0.8416 0.2891 0.0760 1.0000 Uiso R . . . . .
H243 H 0.8021 0.8370 0.3847 0.0760 1.0000 Uiso R . . . . .
H241 H 0.8217 0.8033 0.3275 0.0760 1.0000 Uiso R . . . . .
H251 H 0.7506 0.8818 0.2039 0.0821 1.0000 Uiso R . . . . .
H252 H 0.7088 0.8699 0.2801 0.0820 1.0000 Uiso R . . . . .
H253 H 0.6878 0.8649 0.1458 0.0821 1.0000 Uiso R . . . . .
H262 H 0.4358 0.6247 -0.2235 0.0959 1.0000 Uiso R . . . . .
H263 H 0.3765 0.6424 -0.2963 0.0960 1.0000 Uiso R . . . . .
H261 H 0.4351 0.6451 -0.3368 0.0960 1.0000 Uiso R . . . . .
H281 H 0.3686 0.6891 -0.4155 0.0571 1.0000 Uiso R . . . . .
H291 H 0.3544 0.7440 -0.5090 0.0610 1.0000 Uiso R . . . . .
H301 H 0.3969 0.7941 -0.4183 0.0553 1.0000 Uiso R . . . . .
H331 H 0.4656 0.8210 -0.2639 0.0483 1.0000 Uiso R . . . . .
H341 H 0.5285 0.8518 -0.1416 0.0501 1.0000 Uiso R . . . . .
H342 H 0.5670 0.8317 -0.0305 0.0500 1.0000 Uiso R . . . . .
H361 H 0.5718 0.8950 0.0297 0.0969 1.0000 Uiso R . . . . .
H363 H 0.5308 0.9022 0.1114 0.0969 1.0000 Uiso R . . . . .
H362 H 0.5736 0.8690 0.1311 0.0971 1.0000 Uiso R . . . . .
H372 H 0.9319 0.5984 0.3784 0.2171 1.0000 Uiso R . . . . .
H371 H 0.9256 0.5647 0.4487 0.2170 1.0000 Uiso R . . . . .
H373 H 0.8695 0.5863 0.3863 0.2170 1.0000 Uiso R . . . . .
H411 H 0.8376 0.5314 0.8948 0.1733 0.5000 Uiso R . . . . .
H412 H 0.8704 0.5000 0.8423 0.1733 1.0000 Uiso RS . . . . .
H421 H 0.8827 0.5578 0.7825 0.1920 0.5000 Uiso R . . . . .
H422 H 0.8158 0.5620 0.7366 0.1920 0.5000 Uiso R . . . . .
H423 H 0.8486 0.5346 0.6841 0.1920 0.5000 Uiso R . . . . .
H451 H 0.6950 0.5000 0.7019 0.2274 1.0000 Uiso RS . . . . .
H452 H 0.7300 0.5317 0.6661 0.2274 0.5000 Uiso R . . . . .
H461 H 0.6692 0.5578 0.7799 0.2310 0.5000 Uiso R . . . . .
H462 H 0.6999 0.5324 0.8748 0.2310 0.5000 Uiso R . . . . .
H463 H 0.7348 0.5623 0.8390 0.2310 0.5000 Uiso R . . . . .
H471 H 0.7583 0.5000 0.9231 0.1918 1.0000 Uiso RS . . . . .
H472 H 0.8108 0.4773 0.9399 0.1918 0.5000 Uiso R . . . . .
H481 H 0.7254 0.4488 0.9401 0.1066 0.5000 Uiso R . . . . .
H482 H 0.6951 0.4631 0.8219 0.1066 0.5000 Uiso R . . . . .
H483 H 0.7476 0.4379 0.8386 0.1066 0.5000 Uiso R . . . . .
H432 H 0.7870 0.5000 0.6270 0.1517 1.0000 Uiso RS . . . . .
H441 H 0.8209 0.4391 0.6108 0.1355 0.5000 Uiso R . . . . .
H442 H 0.8226 0.4329 0.7351 0.1355 0.5000 Uiso R . . . . .
H443 H 0.8646 0.4596 0.7044 0.1355 0.5000 Uiso R . . . . .
H391 H 0.5862 0.5663 -0.3587 0.2066 1.0000 Uiso R . . . . .
H392 H 0.5206 0.5744 -0.3772 0.2066 1.0000 Uiso R . . . . .
H393 H 0.5526 0.5503 -0.2795 0.2066 1.0000 Uiso R . . . . .
H431 H 0.7468 0.4704 0.6560 0.1496 0.5000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0807(7) 0.0345(5) 0.0933(7) 0.0000 0.0586(6) 0.0000
Ni1 0.0289(3) 0.0373(4) 0.0234(3) 0.0008(3) 0.0084(3) -0.0034(3)
Ni2 0.0325(5) 0.0362(6) 0.0224(5) 0.0000 0.0085(4) 0.0000
K1 0.0323(7) 0.0423(7) 0.0359(6) -0.0004(6) 0.0092(5) -0.0023(5)
C1 0.064(5) 0.038(4) 0.076(5) -0.008(3) 0.040(4) 0.000(3)
C2 0.121(15) 0.083(11) 0.138(16) 0.0000 0.077(13) 0.0000
C3 0.098(6) 0.037(4) 0.083(6) 0.012(4) 0.053(5) 0.006(4)
C4 0.067(8) 0.052(7) 0.113(11) 0.0000 0.048(8) 0.0000
C5 0.076(5) 0.037(4) 0.078(5) -0.006(4) 0.017(4) 0.003(4)
C6 0.037(3) 0.046(4) 0.036(3) 0.007(3) 0.017(3) -0.002(3)
C7 0.049(4) 0.048(4) 0.053(4) 0.013(3) 0.021(3) 0.007(3)
C8 0.041(4) 0.076(5) 0.045(4) 0.027(4) 0.012(3) 0.016(3)
C9 0.034(3) 0.069(5) 0.036(3) 0.004(3) 0.010(3) 0.003(3)
C10 0.025(3) 0.055(4) 0.026(3) 0.008(3) 0.008(2) 0.002(3)
C11 0.023(3) 0.047(3) 0.030(3) 0.006(3) 0.011(2) -0.003(2)
C12 0.023(3) 0.056(4) 0.026(3) -0.004(3) 0.007(2) -0.006(3)
C13 0.035(3) 0.049(4) 0.034(3) -0.010(3) 0.015(2) -0.007(3)
C14 0.031(3) 0.041(3) 0.043(3) -0.004(3) 0.014(2) -0.005(3)
C15 0.030(3) 0.038(3) 0.045(3) 0.004(3) 0.015(2) -0.003(2)
C16 0.038(3) 0.034(3) 0.041(3) 0.005(3) 0.023(3) 0.005(3)
C17 0.033(3) 0.043(3) 0.026(3) 0.003(3) 0.015(2) 0.004(3)
C18 0.047(4) 0.047(4) 0.040(3) 0.011(3) 0.022(3) 0.013(3)
C19 0.054(4) 0.060(5) 0.038(4) 0.017(3) 0.018(3) 0.019(3)
C20 0.038(3) 0.074(5) 0.025(3) 0.004(3) 0.009(3) 0.013(3)
C21 0.024(3) 0.054(4) 0.025(3) 0.002(3) 0.010(2) 0.003(3)
C22 0.019(2) 0.043(3) 0.023(3) -0.002(2) 0.008(2) 0.004(2)
C23 0.039(3) 0.079(5) 0.028(3) -0.008(3) 0.008(3) -0.012(3)
C24 0.041(4) 0.061(4) 0.049(4) -0.008(3) 0.010(3) -0.012(3)
C25 0.064(4) 0.044(4) 0.054(4) -0.006(3) 0.022(3) -0.001(3)
C26 0.070(5) 0.067(5) 0.060(5) -0.025(4) 0.026(4) -0.019(4)
C27 0.026(3) 0.065(4) 0.030(3) -0.006(3) 0.008(2) 0.003(3)
C28 0.028(3) 0.081(5) 0.033(3) -0.021(3) 0.013(3) -0.010(3)
C29 0.026(3) 0.101(6) 0.027(3) 0.000(4) 0.006(2) 0.010(4)
C30 0.030(3) 0.077(5) 0.029(3) 0.009(3) 0.007(2) 0.011(3)
C31 0.024(3) 0.057(4) 0.027(3) 0.003(3) 0.010(2) 0.007(3)
C32 0.021(3) 0.051(4) 0.027(3) -0.002(3) 0.010(2) 0.003(2)
C33 0.032(3) 0.058(4) 0.037(3) 0.016(3) 0.019(3) 0.013(3)
C34 0.040(3) 0.043(3) 0.043(3) 0.004(3) 0.023(3) 0.002(3)
C35 0.047(5) 0.041(5) 0.043(5) 0.0000 0.028(4) 0.0000
C36 0.074(5) 0.055(4) 0.084(6) -0.020(4) 0.050(4) -0.022(4)
C37 0.204(16) 0.105(10) 0.116(10) -0.022(8) -0.012(10) -0.016(10)
C38 0.154(10) 0.057(6) 0.082(7) -0.001(5) -0.015(7) -0.022(6)
C39 0.229(19) 0.170(15) 0.153(13) -0.052(12) 0.094(13) -0.048(13)
C40 0.111(8) 0.084(7) 0.079(7) -0.013(6) 0.052(6) -0.010(6)
N1 0.070(4) 0.033(3) 0.083(4) -0.001(3) 0.038(3) 0.000(3)
N2 0.094(9) 0.060(6) 0.118(10) 0.0000 0.071(8) 0.0000
N3 0.099(5) 0.040(3) 0.107(6) 0.001(3) 0.071(5) 0.001(3)
N4 0.087(8) 0.037(5) 0.113(9) 0.0000 0.064(7) 0.0000
N5 0.029(2) 0.040(3) 0.028(2) -0.003(2) 0.0130(19) -0.010(2)
N6 0.031(2) 0.039(3) 0.031(2) -0.002(2) 0.013(2) -0.005(2)
N7 0.034(3) 0.040(3) 0.029(2) 0.006(2) 0.013(2) 0.005(2)
N8 0.283(16) 0.078(7) 0.083(7) -0.016(5) -0.007(8) -0.047(8)
N9 0.097(6) 0.092(6) 0.085(6) -0.003(5) 0.033(5) 0.002(5)
O1 0.048(2) 0.036(2) 0.042(2) 0.0004(19) 0.0116(19) 0.0004(19)
O2 0.038(2) 0.036(2) 0.0250(19) 0.0047(17) 0.0055(16) -0.0050(17)
O3 0.035(2) 0.039(2) 0.0212(18) 0.0003(17) 0.0023(15) -0.0024(17)
O4 0.037(2) 0.050(3) 0.029(2) -0.0057(18) 0.0067(17) -0.0066(18)
O5 0.048(3) 0.051(3) 0.039(2) -0.015(2) 0.0110(19) -0.007(2)
O6 0.035(2) 0.043(2) 0.0196(18) -0.0022(16) 0.0006(15) 0.0028(17)
S1 0.128(2) 0.0556(12) 0.1056(18) 0.0030(12) 0.0792(17) -0.0166(13)
S2 0.149(5) 0.210(7) 0.166(6) 0.0000 0.013(5) 0.0000
S3 0.177(3) 0.0580(13) 0.112(2) 0.0137(14) 0.098(2) 0.0389(16)
S4 0.096(3) 0.122(4) 0.149(4) 0.0000 0.035(3) 0.0000
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 . N3 6_565 2.074(6) yes
Mo1 . N1 6_565 2.071(6) yes
Mo1 . N1 . 2.071(6) yes
Mo1 . N2 . 2.012(15) yes
Mo1 . N3 . 2.074(6) yes
Mo1 . N4 . 2.099(14) yes
Ni1 . N5 . 1.848(4) yes
Ni1 . N6 . 1.851(5) yes
Ni1 . O2 . 1.833(4) yes
Ni1 . O3 . 1.824(3) yes
Ni2 . N7 5_655 1.848(4) yes
Ni2 . O6 5_655 1.835(4) yes
Ni2 . N7 . 1.848(4) yes
Ni2 . O6 . 1.835(4) yes
C1 . N1 . 1.151(8) yes
C1 . S1 . 1.598(7) yes
C2 . N2 . 1.13(2) yes
C2 . S2 . 1.64(2) yes
C3 . N3 . 1.143(9) yes
C3 . S3 . 1.610(8) yes
C4 . N4 . 1.132(16) yes
C4 . S4 . 1.621(17) yes
C5 . O1 . 1.416(8) yes
C5 . H51 . 0.963 no
C5 . H53 . 0.961 no
C5 . H52 . 0.959 no
C6 . C7 . 1.353(8) yes
C6 . C11 . 1.413(8) yes
C6 . O1 . 1.354(7) yes
C7 . C8 . 1.394(10) yes
C7 . H71 . 0.930 no
C8 . C9 . 1.348(10) yes
C8 . H81 . 0.929 no
C9 . C10 . 1.391(8) yes
C9 . H91 . 0.937 no
C10 . C11 . 1.400(8) yes
C10 . C12 . 1.418(9) yes
C11 . O2 . 1.293(6) yes
C12 . N5 . 1.264(7) yes
C12 . H121 . 0.936 no
C13 . C14 . 1.519(8) yes
C13 . N5 . 1.452(7) yes
C13 . H131 . 0.977 no
C13 . H132 . 0.972 no
C14 . C15 . 1.508(8) yes
C14 . C24 . 1.516(8) yes
C14 . C25 . 1.510(9) yes
C15 . N6 . 1.466(7) yes
C15 . H151 . 0.967 no
C15 . H152 . 0.973 no
C16 . C17 . 1.418(8) yes
C16 . N6 . 1.272(7) yes
C16 . H161 . 0.940 no
C17 . C18 . 1.383(8) yes
C17 . C22 . 1.403(8) yes
C18 . C19 . 1.356(9) yes
C18 . H181 . 0.936 no
C19 . C20 . 1.370(10) yes
C19 . H191 . 0.934 no
C20 . C21 . 1.365(8) yes
C20 . H201 . 0.935 no
C21 . C22 . 1.408(7) yes
C21 . O4 . 1.361(7) yes
C22 . O3 . 1.294(6) yes
C23 . O4 . 1.413(7) yes
C23 . H231 . 0.965 no
C23 . H232 . 0.967 no
C23 . H233 . 0.968 no
C24 . H242 . 0.963 no
C24 . H243 . 0.961 no
C24 . H241 . 0.960 no
C25 . H251 . 0.965 no
C25 . H252 . 0.972 no
C25 . H253 . 0.964 no
C26 . O5 . 1.418(8) yes
C26 . H262 . 0.954 no
C26 . H263 . 0.969 no
C26 . H261 . 0.965 no
C27 . C28 . 1.367(8) yes
C27 . C32 . 1.408(8) yes
C27 . O5 . 1.362(8) yes
C28 . C29 . 1.393(10) yes
C28 . H281 . 0.936 no
C29 . C30 . 1.338(10) yes
C29 . H291 . 0.928 no
C30 . C31 . 1.395(8) yes
C30 . H301 . 0.941 no
C31 . C32 . 1.377(8) yes
C31 . C33 . 1.418(9) yes
C32 . O6 . 1.302(6) yes
C33 . N7 . 1.278(7) yes
C33 . H331 . 0.928 no
C34 . C35 . 1.513(7) yes
C34 . N7 . 1.453(7) yes
C34 . H341 . 0.975 no
C34 . H342 . 0.978 no
C35 . C36 5_655 1.509(9) yes
C35 . C36 . 1.509(9) yes
C36 . H361 . 0.959 no
C36 . H363 . 0.955 no
C36 . H362 . 0.958 no
C37 . C38 . 1.411(16) yes
C37 . H372 . 0.962 no
C37 . H371 . 0.959 no
C37 . H373 . 0.957 no
C38 . N8 . 1.075(13) yes
C39 . C40 . 1.422(17) yes
C39 . H391 . 0.930 no
C39 . H392 . 0.930 no
C39 . H393 . 0.930 no
C40 . N9 . 1.076(11) yes
C41 . C42 . 1.40(3) yes
C41 . N10 . 1.47(2) yes
C41 . H411 . 0.921 no
C41 . H412 . 1.065 no
C42 . H421 . 0.889 no
C42 . H422 . 0.943 no
C42 . H423 . 0.931 no
C43 . C43 6_565 1.5186(8) yes
C43 . C45 6_565 1.57(4) yes
C43 . H452 6_565 1.282 no
C43 . C44 . 1.53(2) yes
C43 . N10 . 1.44(2) yes
C43 . H432 . 1.037 no
C43 . H431 . 0.900 no
C44 . H441 . 0.929 no
C44 . H442 . 0.925 no
C44 . H443 . 0.918 no
C45 . H431 6_565 1.164 no
C45 . C45 6_565 1.3664(8) yes
C45 . C46 . 1.60(3) yes
C45 . N10 . 1.49(3) yes
C45 . H451 . 0.975 no
C45 . H452 . 0.905 no
C46 . H483 6_565 1.117 no
C46 . C48 6_565 0.81(4) yes
C46 . H461 . 0.957 no
C46 . H462 . 0.993 no
C46 . H463 . 0.911 no
C47 . C47 6_565 1.1525(8) yes
C47 . C48 . 1.45(2) yes
C47 . N10 . 1.48(2) yes
C47 . H471 . 0.850 no
C47 . H472 . 0.939 no
C48 . H481 . 0.927 no
C48 . H482 . 0.915 no
C48 . H483 . 0.932 no
H452 . H431 6_565 0.448 no
H462 . H482 6_565 0.645 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 6_565 Mo1 . N1 6_565 91.3(2) yes
N3 6_565 Mo1 . N1 . 179.2(3) yes
N1 6_565 Mo1 . N1 . 89.2(3) yes
N3 6_565 Mo1 . N2 . 90.2(3) yes
N1 6_565 Mo1 . N2 . 89.2(3) yes
N1 . Mo1 . N2 . 89.2(3) yes
N3 6_565 Mo1 . N3 . 88.2(3) yes
N1 6_565 Mo1 . N3 . 179.2(3) yes
N1 . Mo1 . N3 . 91.3(2) yes
N2 . Mo1 . N3 . 90.2(3) yes
N3 6_565 Mo1 . N4 . 92.1(3) yes
N1 6_565 Mo1 . N4 . 88.5(3) yes
N1 . Mo1 . N4 . 88.5(3) yes
N2 . Mo1 . N4 . 176.8(4) yes
N3 . Mo1 . N4 . 92.1(3) yes
N5 . Ni1 . N6 . 91.31(19) yes
N5 . Ni1 . O2 . 92.75(18) yes
N6 . Ni1 . O2 . 169.24(18) yes
N5 . Ni1 . O3 . 168.09(17) yes
N6 . Ni1 . O3 . 94.44(18) yes
O2 . Ni1 . O3 . 83.46(16) yes
N7 5_655 Ni2 . O6 5_655 94.68(18) yes
N7 5_655 Ni2 . N7 . 90.1(3) yes
O6 5_655 Ni2 . N7 . 167.21(18) yes
N7 5_655 Ni2 . O6 . 167.21(18) yes
O6 5_655 Ni2 . O6 . 83.1(2) yes
N7 . Ni2 . O6 . 94.68(18) yes
N1 . C1 . S1 . 179.5(6) yes
N2 . C2 . S2 . 179.5(17) yes
N3 . C3 . S3 . 178.0(9) yes
N4 . C4 . S4 . 178.5(12) yes
O1 . C5 . H51 . 108.9 no
O1 . C5 . H53 . 108.9 no
H51 . C5 . H53 . 109.9 no
O1 . C5 . H52 . 109.2 no
H51 . C5 . H52 . 110.5 no
H53 . C5 . H52 . 109.4 no
C7 . C6 . C11 . 120.9(6) yes
C7 . C6 . O1 . 125.4(6) yes
C11 . C6 . O1 . 113.7(5) yes
C6 . C7 . C8 . 121.3(7) yes
C6 . C7 . H71 . 119.1 no
C8 . C7 . H71 . 119.6 no
C7 . C8 . C9 . 118.9(6) yes
C7 . C8 . H81 . 120.0 no
C9 . C8 . H81 . 121.1 no
C8 . C9 . C10 . 121.3(6) yes
C8 . C9 . H91 . 119.7 no
C10 . C9 . H91 . 119.0 no
C9 . C10 . C11 . 120.6(6) yes
C9 . C10 . C12 . 120.2(5) yes
C11 . C10 . C12 . 119.0(5) yes
C6 . C11 . C10 . 116.9(5) yes
C6 . C11 . O2 . 118.5(5) yes
C10 . C11 . O2 . 124.5(5) yes
C10 . C12 . N5 . 126.1(5) yes
C10 . C12 . H121 . 116.7 no
N5 . C12 . H121 . 117.3 no
C14 . C13 . N5 . 112.5(4) yes
C14 . C13 . H131 . 109.8 no
N5 . C13 . H131 . 109.4 no
C14 . C13 . H132 . 107.8 no
N5 . C13 . H132 . 107.7 no
H131 . C13 . H132 . 109.5 no
C13 . C14 . C15 . 110.1(5) yes
C13 . C14 . C24 . 108.9(5) yes
C15 . C14 . C24 . 107.9(5) yes
C13 . C14 . C25 . 108.4(5) yes
C15 . C14 . C25 . 111.3(5) yes
C24 . C14 . C25 . 110.3(5) yes
C14 . C15 . N6 . 113.3(4) yes
C14 . C15 . H151 . 108.1 no
N6 . C15 . H151 . 108.9 no
C14 . C15 . H152 . 108.8 no
N6 . C15 . H152 . 108.5 no
H151 . C15 . H152 . 109.1 no
C17 . C16 . N6 . 126.7(5) yes
C17 . C16 . H161 . 116.5 no
N6 . C16 . H161 . 116.7 no
C16 . C17 . C18 . 119.2(6) yes
C16 . C17 . C22 . 119.9(5) yes
C18 . C17 . C22 . 120.7(5) yes
C17 . C18 . C19 . 120.9(6) yes
C17 . C18 . H181 . 118.7 no
C19 . C18 . H181 . 120.4 no
C18 . C19 . C20 . 119.5(6) yes
C18 . C19 . H191 . 120.3 no
C20 . C19 . H191 . 120.2 no
C19 . C20 . C21 . 121.2(6) yes
C19 . C20 . H201 . 120.3 no
C21 . C20 . H201 . 118.5 no
C20 . C21 . C22 . 120.8(6) yes
C20 . C21 . O4 . 125.5(5) yes
C22 . C21 . O4 . 113.7(5) yes
C21 . C22 . C17 . 116.8(5) yes
C21 . C22 . O3 . 118.8(5) yes
C17 . C22 . O3 . 124.3(5) yes
O4 . C23 . H231 . 108.3 no
O4 . C23 . H232 . 110.3 no
H231 . C23 . H232 . 110.3 no
O4 . C23 . H233 . 109.1 no
H231 . C23 . H233 . 109.6 no
H232 . C23 . H233 . 109.1 no
C14 . C24 . H242 . 109.0 no
C14 . C24 . H243 . 109.6 no
H242 . C24 . H243 . 110.2 no
C14 . C24 . H241 . 109.0 no
H242 . C24 . H241 . 109.6 no
H243 . C24 . H241 . 109.4 no
C14 . C25 . H251 . 109.7 no
C14 . C25 . H252 . 109.3 no
H251 . C25 . H252 . 109.3 no
C14 . C25 . H253 . 108.9 no
H251 . C25 . H253 . 109.8 no
H252 . C25 . H253 . 109.8 no
O5 . C26 . H262 . 108.9 no
O5 . C26 . H263 . 109.7 no
H262 . C26 . H263 . 110.1 no
O5 . C26 . H261 . 108.7 no
H262 . C26 . H261 . 110.0 no
H263 . C26 . H261 . 109.3 no
C28 . C27 . C32 . 120.6(6) yes
C28 . C27 . O5 . 125.0(6) yes
C32 . C27 . O5 . 114.4(5) yes
C27 . C28 . C29 . 120.3(6) yes
C27 . C28 . H281 . 119.5 no
C29 . C28 . H281 . 120.2 no
C28 . C29 . C30 . 120.1(6) yes
C28 . C29 . H291 . 120.1 no
C30 . C29 . H291 . 119.8 no
C29 . C30 . C31 . 120.1(6) yes
C29 . C30 . H301 . 119.8 no
C31 . C30 . H301 . 120.1 no
C30 . C31 . C32 . 121.5(6) yes
C30 . C31 . C33 . 117.8(6) yes
C32 . C31 . C33 . 120.4(5) yes
C27 . C32 . C31 . 117.3(5) yes
C27 . C32 . O6 . 117.3(5) yes
C31 . C32 . O6 . 125.4(5) yes
C31 . C33 . N7 . 125.9(5) yes
C31 . C33 . H331 . 117.0 no
N7 . C33 . H331 . 117.1 no
C35 . C34 . N7 . 113.1(4) yes
C35 . C34 . H341 . 108.4 no
N7 . C34 . H341 . 108.8 no
C35 . C34 . H342 . 108.3 no
N7 . C34 . H342 . 108.5 no
H341 . C34 . H342 . 109.7 no
C34 . C35 . C34 5_655 108.5(7) yes
C34 . C35 . C36 5_655 109.3(4) yes
C34 5_655 C35 . C36 5_655 108.8(4) yes
C34 . C35 . C36 . 108.8(4) yes
C34 5_655 C35 . C36 . 109.3(4) yes
C36 5_655 C35 . C36 . 112.1(9) yes
C35 . C36 . H361 . 109.5 no
C35 . C36 . H363 . 108.6 no
H361 . C36 . H363 . 111.1 no
C35 . C36 . H362 . 108.0 no
H361 . C36 . H362 . 109.1 no
H363 . C36 . H362 . 110.5 no
C38 . C37 . H372 . 109.3 no
C38 . C37 . H371 . 111.2 no
H372 . C37 . H371 . 107.9 no
C38 . C37 . H373 . 111.9 no
H372 . C37 . H373 . 108.1 no
H371 . C37 . H373 . 108.2 no
C37 . C38 . N8 . 174.7(15) yes
C40 . C39 . H391 . 109.7 no
C40 . C39 . H392 . 109.1 no
H391 . C39 . H392 . 109.5 no
C40 . C39 . H393 . 109.5 no
H391 . C39 . H393 . 109.5 no
H392 . C39 . H393 . 109.5 no
C39 . C40 . N9 . 177.1(12) yes
Mo1 . N1 . C1 . 176.1(5) yes
Mo1 . N2 . C2 . 168.6(13) yes
Mo1 . N3 . C3 . 174.7(6) yes
Mo1 . N4 . C4 . 170.7(10) yes
C13 . N5 . C12 . 118.4(5) yes
C13 . N5 . Ni1 . 115.4(4) yes
C12 . N5 . Ni1 . 125.8(4) yes
C15 . N6 . C16 . 118.2(5) yes
C15 . N6 . Ni1 . 116.0(4) yes
C16 . N6 . Ni1 . 125.1(4) yes
C34 . N7 . C33 . 119.1(5) yes
C34 . N7 . Ni2 . 115.9(4) yes
C33 . N7 . Ni2 . 124.6(4) yes
C5 . O1 . C6 . 116.7(5) yes
C11 . O2 . Ni1 . 125.3(4) yes
C22 . O3 . Ni1 . 127.1(3) yes
C23 . O4 . C21 . 115.9(5) yes
C26 . O5 . C27 . 116.1(5) yes
C32 . O6 . Ni2 . 124.2(4) yes
C42 . C41 . N10 . 115(2) yes
C42 . C41 . H411 . 109.1 no
N10 . C41 . H411 . 110.0 no
C42 . C41 . H412 . 111.5 no
N10 . C41 . H412 . 101.5 no
H411 . C41 . H412 . 109.6 no
C41 . C42 . H421 . 110.7 no
C41 . C42 . H422 . 105.5 no
H421 . C42 . H422 . 111.9 no
C41 . C42 . H423 . 106.8 no
H421 . C42 . H423 . 113.1 no
H422 . C42 . H423 . 108.3 no
C43 6_565 C43 . C45 6_565 87.22(7) yes
C43 6_565 C43 . H452 6_565 109.5 no
C43 6_565 C43 . C44 . 137.6(12) yes
C45 6_565 C43 . C44 . 132.5(13) yes
H452 6_565 C43 . C44 . 112.4 no
C43 6_565 C43 . N10 . 58.2(5) yes
C45 6_565 C43 . N10 . 59.4(12) yes
H452 6_565 C43 . N10 . 94.5 no
C44 . C43 . N10 . 123.6(19) yes
C45 6_565 C43 . H432 . 114.2 no
H452 6_565 C43 . H432 . 112.9 no
C44 . C43 . H432 . 111.3 no
N10 . C43 . H432 . 100.9 no
C43 6_565 C43 . H431 . 112.9 no
C44 . C43 . H431 . 106.6 no
N10 . C43 . H431 . 106.6 no
H432 . C43 . H431 . 106.7 no
C43 . C44 . H441 . 111.9 no
C43 . C44 . H442 . 106.7 no
H441 . C44 . H442 . 110.1 no
C43 . C44 . H443 . 106.3 no
H441 . C44 . H443 . 110.7 no
H442 . C44 . H443 . 111.1 no
C43 6_565 C45 . C45 6_565 92.78(7) yes
H431 6_565 C45 . C45 6_565 111.5 no
C43 6_565 C45 . C46 . 126(2) yes
H431 6_565 C45 . C46 . 118.0 no
C45 6_565 C45 . C46 . 130.3(16) yes
C43 6_565 C45 . N10 . 56.0(13) yes
H431 6_565 C45 . N10 . 90.6 no
C45 6_565 C45 . N10 . 62.8(5) yes
C46 . C45 . N10 . 111(2) yes
C43 6_565 C45 . H451 . 124.6 no
H431 6_565 C45 . H451 . 117.9 no
C46 . C45 . H451 . 109.0 no
N10 . C45 . H451 . 108.0 no
C43 6_565 C45 . H452 . 54.8 no
C45 6_565 C45 . H452 . 123.9 no
C46 . C45 . H452 . 104.8 no
N10 . C45 . H452 . 110.7 no
H451 . C45 . H452 . 113.0 no
H483 6_565 C46 . C45 . 101.1 no
H483 6_565 C46 . C48 6_565 55.0 no
C45 . C46 . C48 6_565 106(4) yes
H483 6_565 C46 . H461 . 118.8 no
C45 . C46 . H461 . 117.1 no
C48 6_565 C46 . H461 . 135.9 no
H483 6_565 C46 . H462 . 108.7 no
C45 . C46 . H462 . 108.5 no
C48 6_565 C46 . H462 . 54.8 no
H461 . C46 . H462 . 102.3 no
C45 . C46 . H463 . 113.3 no
C48 6_565 C46 . H463 . 56.0 no
H461 . C46 . H463 . 108.8 no
H462 . C46 . H463 . 105.8 no
C47 6_565 C47 . C48 . 137.0(12) yes
C47 6_565 C47 . N10 . 67.1(4) yes
C48 . C47 . N10 . 113.3(19) yes
C47 6_565 C47 . H471 . 47.3 no
C48 . C47 . H471 . 100.6 no
N10 . C47 . H471 . 109.4 no
C47 6_565 C47 . H472 . 106.9 no
C48 . C47 . H472 . 111.5 no
N10 . C47 . H472 . 111.9 no
H471 . C47 . H472 . 109.4 no
C47 . C48 . C46 6_565 120(4) yes
C47 . C48 . H481 . 109.4 no
C46 6_565 C48 . H481 . 125.9 no
C47 . C48 . H482 . 112.0 no
H481 . C48 . H482 . 111.0 no
C47 . C48 . H483 . 103.9 no
C46 6_565 C48 . H483 . 79.3 no
H481 . C48 . H483 . 109.6 no
H482 . C48 . H483 . 110.7 no
C45 . N10 . C45 6_565 54.4(10) yes
C45 . N10 . C47 . 106.4(17) yes
C45 6_565 N10 . C47 . 85.8(16) yes
C45 . N10 . C47 6_565 85.8(16) yes
C45 6_565 N10 . C47 6_565 106.4(17) yes
C45 . N10 . C41 6_565 172.8(16) yes
C45 6_565 N10 . C41 6_565 120.8(8) yes
C47 . N10 . C41 6_565 77.6(15) yes
C47 6_565 N10 . C41 6_565 101.2(16) yes
C45 . N10 . C41 . 120.8(8) yes
C45 6_565 N10 . C41 . 172.8(16) yes
C47 . N10 . C41 . 101.2(16) yes
C47 6_565 N10 . C41 . 77.6(15) yes
C41 6_565 N10 . C41 . 63.2(11) yes
C45 . N10 . C43 . 93.0(14) yes
C45 6_565 N10 . C43 . 64.6(14) yes
C47 . N10 . C43 . 124.8(6) yes
C47 6_565 N10 . C43 . 169.1(11) yes
C41 6_565 N10 . C43 . 79.8(14) yes
C45 . N10 . C43 6_565 64.6(14) yes
C45 6_565 N10 . C43 6_565 93.0(14) yes
C47 . N10 . C43 6_565 169.1(11) yes
C47 6_565 N10 . C43 6_565 124.8(6) yes
C41 6_565 N10 . C43 6_565 112.0(16) yes
C41 . N10 . C43 . 112.0(16) yes
C41 . N10 . C43 6_565 79.8(14) yes
C43 . N10 . C43 6_565 63.6(10) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C15 . H152 . O3 4_665 151 0.97 2.39 3.270(7) yes
C33 . H331 . N8 8_464 160 0.93 2.55 3.434(15) yes
C47 6_565 H471 . C48 . 128 0.85 1.81 2.428(15) yes
C47 . H471 . C48 6_565 128 0.85 1.81 2.428(15) yes
C43 . H432 . C44 6_565 123 1.04 2.14 2.843(15) yes
C43 6_565 H432 . C44 . 123 1.04 2.14 2.843(15) yes
C45 6_565 H431 . C44 . 127 1.16 1.99 2.838(15) yes
# Attachment '3908_web_deposit_cif_file_2_Jean-PascalSutter_1295611074.cif'
data_cpd3
_database_code_depnum_ccdc_archive 'CCDC 809269'
#TrackingRef '3908_web_deposit_cif_file_2_Jean-PascalSutter_1295611074.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details
;
?
;
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 23.4893(11)
_cell_length_b 33.2913(15)
_cell_length_c 15.1039(6)
_cell_angle_alpha 90
_cell_angle_beta 116.265(2)
_cell_angle_gamma 90
_cell_volume 10591.7(8)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 1 2/c 1 '
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mo -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584
4.3875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240
0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C98 H116 Mo1 N15 Na2 Ni4 O16 S6
# Dc = 1.46 Fooo = 4836.00 Mu = 10.09 M = 1164.62
# Found Formula = C98 H116 Mo1 N15 Na2 Ni4 O16 S6
# Dc = 1.46 FOOO = 4836.00 Mu = 10.09 M = 1164.62
_chemical_formula_sum 'C98 H116 Mo1 N15 Na2 Ni4 O16 S6'
_chemical_formula_moiety '2(C42 H48 N4 Na Ni2 O8),C8 H20 N,C6 Mo N6 S6 '
_chemical_compound_source ?
_chemical_formula_weight 2329.25
_cell_measurement_reflns_used 9890
_cell_measurement_theta_min 2
_cell_measurement_theta_max 32
_cell_measurement_temperature 180
_exptl_crystal_description planar
_exptl_crystal_colour orange
_exptl_crystal_size_min 0.050
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_max 0.300
_exptl_crystal_density_diffrn 1.461
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 4836
_exptl_absorpt_coefficient_mu 1.009
# Sheldrick geometric approximatio 0.74 0.95
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min 0.89
_exptl_absorpt_correction_T_max 0.95
_diffrn_measurement_device-type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 180
_diffrn_reflns_number 142585
_reflns_number_total 18759
_diffrn_reflns_av_R_equivalents 0.040
# Number of reflections without Friedels Law is 18759
# Number of reflections with Friedels Law is 0
# Theoretical number of reflections is about 18817
_diffrn_reflns_theta_min 1.144
_diffrn_reflns_theta_max 32.285
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 32.285
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_h_max 35
_diffrn_reflns_limit_k_min -50
_diffrn_reflns_limit_k_max 50
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 22
_reflns_limit_h_min -35
_reflns_limit_h_max 31
_reflns_limit_k_min 0
_reflns_limit_k_max 50
_reflns_limit_l_min 0
_reflns_limit_l_max 22
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.62
_refine_diff_density_max 1.04
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 11492
_refine_ls_number_restraints 4
_refine_ls_number_parameters 635
_oxford_refine_ls_R_factor_ref 0.0364
_refine_ls_wR_factor_ref 0.0392
_refine_ls_goodness_of_fit_ref 1.0906
_refine_ls_shift/su_max 0.0003213
_refine_ls_shift/su_mean 0.0000961
# The values computed from all data
_oxford_reflns_number_all 18716
_refine_ls_R_factor_all 0.0766
_refine_ls_wR_factor_all 0.0830
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 12525
_refine_ls_R_factor_gt 0.0400
_refine_ls_wR_factor_gt 0.0414
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.492 0.255 0.221
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Mo1 Mo 0.7500 0.7500 0.5000 0.0324 1.0000 Uani S . . . . . .
Ni1 Ni 0.683380(12) 0.540286(7) 0.373737(18) 0.0222 1.0000 Uani . . . . . . .
Ni2 Ni 0.796094(13) 0.361384(8) 0.58931(2) 0.0274 1.0000 Uani . . . . . . .
C1 C 0.81201(11) 0.72400(7) 0.73201(19) 0.0343 1.0000 Uani . . . . . . .
C2 C 0.80771(10) 0.66666(7) 0.45752(17) 0.0330 1.0000 Uani . . . . . . .
C3 C 0.62631(11) 0.70847(7) 0.50227(17) 0.0323 1.0000 Uani . . . . . . .
C4 C 0.70820(16) 0.36772(7) 0.3270(2) 0.0472 1.0000 Uani . . . . . . .
C5 C 0.66268(11) 0.42914(6) 0.24703(16) 0.0304 1.0000 Uani . . . . . . .
C6 C 0.62417(12) 0.40984(7) 0.15999(18) 0.0379 1.0000 Uani . . . . . . .
C7 C 0.58646(12) 0.43196(8) 0.07586(18) 0.0412 1.0000 Uani . . . . . . .
C8 C 0.58834(12) 0.47292(8) 0.07820(17) 0.0382 1.0000 Uani . . . . . . .
C9 C 0.62611(10) 0.49335(6) 0.16705(15) 0.0293 1.0000 Uani . . . . . . .
C10 C 0.66234(10) 0.47176(6) 0.25394(15) 0.0265 1.0000 Uani . . . . . . .
C11 C 0.63202(10) 0.53625(7) 0.16687(15) 0.0297 1.0000 Uani . . . . . . .
C12 C 0.66402(10) 0.60167(6) 0.23284(15) 0.0278 1.0000 Uani . . . . . . .
C13 C 0.61586(10) 0.62698(6) 0.25106(15) 0.0266 1.0000 Uani . . . . . . .
C14 C 0.61129(10) 0.61215(6) 0.34394(16) 0.0298 1.0000 Uani . . . . . . .
C15 C 0.69983(10) 0.60533(6) 0.50147(15) 0.0278 1.0000 Uani . . . . . . .
C16 C 0.74573(10) 0.58361(6) 0.58416(15) 0.0275 1.0000 Uani . . . . . . .
C17 C 0.78301(12) 0.60388(7) 0.67349(17) 0.0359 1.0000 Uani . . . . . . .
C18 C 0.81814(13) 0.58270(8) 0.75781(18) 0.0435 1.0000 Uani . . . . . . .
C19 C 0.81592(12) 0.54059(8) 0.75698(16) 0.0379 1.0000 Uani . . . . . . .
C20 C 0.78000(10) 0.52017(6) 0.67096(15) 0.0294 1.0000 Uani . . . . . . .
C21 C 0.74549(9) 0.54146(6) 0.58111(14) 0.0255 1.0000 Uani . . . . . . .
C22 C 0.80499(14) 0.45577(8) 0.74726(18) 0.0450 1.0000 Uani . . . . . . .
C23 C 0.63759(13) 0.67069(7) 0.2642(2) 0.0405 1.0000 Uani . . . . . . .
C24 C 0.55036(12) 0.62350(9) 0.16313(18) 0.0426 1.0000 Uani . . . . . . .
C25 C 0.86582(14) 0.52295(7) 0.5235(2) 0.0449 1.0000 Uani . . . . . . .
C26 C 0.89998(11) 0.45501(8) 0.5561(2) 0.0424 1.0000 Uani . . . . . . .
C27 C 0.95973(14) 0.46372(10) 0.5662(3) 0.0689 1.0000 Uani . . . . . . .
C28 C 1.00603(16) 0.43337(13) 0.5886(4) 0.0988 1.0000 Uani . . . . . . .
C29 C 0.99217(16) 0.39497(12) 0.6021(4) 0.0907 1.0000 Uani . . . . . . .
C30 C 0.93128(13) 0.38517(9) 0.5941(3) 0.0553 1.0000 Uani . . . . . . .
C31 C 0.88426(11) 0.41498(7) 0.57096(19) 0.0373 1.0000 Uani . . . . . . .
C32 C 0.91799(13) 0.34429(8) 0.6062(3) 0.0525 1.0000 Uani . . . . . . .
C33 C 0.86185(13) 0.28699(7) 0.61219(19) 0.0387 1.0000 Uani . . . . . . .
C34 C 0.85735(12) 0.27278(6) 0.70542(18) 0.0348 1.0000 Uani . . . . . . .
C35 C 0.80867(14) 0.29806(7) 0.72290(18) 0.0420 1.0000 Uani . . . . . . .
C36 C 0.70440(13) 0.30898(6) 0.59468(19) 0.0375 1.0000 Uani . . . . . . .
C37 C 0.65409(12) 0.33155(7) 0.51942(19) 0.0356 1.0000 Uani . . . . . . .
C38 C 0.59263(13) 0.31479(8) 0.4695(2) 0.0441 1.0000 Uani . . . . . . .
C39 C 0.54346(13) 0.33682(9) 0.4043(2) 0.0465 1.0000 Uani . . . . . . .
C40 C 0.55206(11) 0.37764(8) 0.39076(18) 0.0393 1.0000 Uani . . . . . . .
C41 C 0.61099(11) 0.39538(7) 0.44182(16) 0.0313 1.0000 Uani . . . . . . .
C42 C 0.66462(10) 0.37221(6) 0.50433(16) 0.0290 1.0000 Uani . . . . . . .
C43 C 0.57251(11) 0.45972(8) 0.37149(19) 0.0397 1.0000 Uani . . . . . . .
C44 C 0.83702(15) 0.22890(7) 0.6899(2) 0.0469 1.0000 Uani . . . . . . .
C45 C 0.92182(16) 0.27618(10) 0.7957(2) 0.0584 1.0000 Uani . . . . . . .
N1 N 0.79287(10) 0.73562(6) 0.65128(16) 0.0378 1.0000 Uani . . . . . . .
N2 N 0.78575(10) 0.69563(6) 0.47314(16) 0.0391 1.0000 Uani . . . . . . .
N3 N 0.66805(10) 0.72195(6) 0.49125(16) 0.0393 1.0000 Uani . . . . . . .
N4 N 0.65574(8) 0.55851(5) 0.24477(12) 0.0260 1.0000 Uani . . . . . . .
N5 N 0.66804(8) 0.59042(5) 0.41426(12) 0.0249 1.0000 Uani . . . . . . .
N6 N 0.86729(10) 0.33086(6) 0.60816(16) 0.0365 1.0000 Uani . . . . . . .
N7 N 0.76358(10) 0.31902(5) 0.63352(14) 0.0334 1.0000 Uani . . . . . . .
O1 O 0.70322(9) 0.41040(4) 0.33235(12) 0.0371 1.0000 Uani . . . . . . .
O2 O 0.69639(7) 0.48874(4) 0.34024(10) 0.0280 1.0000 Uani . . . . . . .
O3 O 0.71449(7) 0.52017(4) 0.50033(10) 0.0280 1.0000 Uani . . . . . . .
O4 O 0.77285(8) 0.47940(5) 0.66079(11) 0.0354 1.0000 Uani . . . . . . .
O5 O 0.85128(8) 0.48188(5) 0.53042(14) 0.0394 1.0000 Uani . . . . . . .
O6 O 0.82665(7) 0.40786(4) 0.55900(12) 0.0317 1.0000 Uani . . . . . . .
O7 O 0.72028(7) 0.38994(4) 0.54794(11) 0.0286 1.0000 Uani . . . . . . .
O8 O 0.62344(7) 0.43533(5) 0.43820(12) 0.0335 1.0000 Uani . . . . . . .
S1 S 0.83889(4) 0.70740(2) 0.84483(5) 0.0469 1.0000 Uani . . . . . . .
S2 S 0.83742(3) 0.62633(2) 0.43405(5) 0.0445 1.0000 Uani . . . . . . .
S3 S 0.56771(3) 0.68904(2) 0.51616(6) 0.0483 1.0000 Uani . . . . . . .
Na1 Na 0.74006(4) 0.45250(2) 0.48974(6) 0.0282 1.0000 Uani . . . . . . .
N8 N 1.0000 0.32318(12) 0.2500 0.0574(9) 1.0000 Uiso S . . . . . .
C46 C 1.0491(4) 0.3560(3) 0.2597(7) 0.075(2) 0.5000 Uiso . . . . . . .
C47 C 1.018324(10) 0.3968(3) 0.215162(10) 0.117(4) 0.5000 Uiso . . . . . . .
C48 C 0.9537(3) 0.31823(19) 0.1427(4) 0.0506(13) 0.5000 Uiso . . . . . . .
C49 C 0.9841(3) 0.3075(2) 0.0747(5) 0.0580(15) 0.5000 Uiso . . . . . . .
C50 C 1.0361(4) 0.2854(3) 0.2894(7) 0.086(2) 0.5000 Uiso . . . . . . .
C51 C 1.000000(10) 0.2464(4) 0.250000(10) 0.217(6) 1.0000 Uiso S . . . . . .
C52 C 0.9587(5) 0.3356(3) 0.2985(7) 0.088(3) 0.5000 Uiso . . . . . . .
C53 C 0.9923(9) 0.3450(6) 0.4072(13) 0.188(7) 0.5000 Uiso . . . . . . .
H43 H 0.7425 0.3585 0.3886 0.0738 1.0000 Uiso R . . . . . .
H42 H 0.7184 0.3614 0.2734 0.0733 1.0000 Uiso R . . . . . .
H41 H 0.6678 0.3553 0.3144 0.0743 1.0000 Uiso R . . . . . .
H61 H 0.6236 0.3815 0.1566 0.0467 1.0000 Uiso R . . . . . .
H71 H 0.5602 0.4183 0.0177 0.0508 1.0000 Uiso R . . . . . .
H81 H 0.5649 0.4879 0.0203 0.0476 1.0000 Uiso R . . . . . .
H111 H 0.6185 0.5492 0.1048 0.0359 1.0000 Uiso R . . . . . .
H122 H 0.7066 0.6095 0.2805 0.0336 1.0000 Uiso R . . . . . .
H121 H 0.6590 0.6066 0.1658 0.0341 1.0000 Uiso R . . . . . .
H141 H 0.6036 0.6351 0.3773 0.0373 1.0000 Uiso R . . . . . .
H142 H 0.5754 0.5934 0.3240 0.0368 1.0000 Uiso R . . . . . .
H151 H 0.6908 0.6326 0.5121 0.0340 1.0000 Uiso R . . . . . .
H171 H 0.7828 0.6322 0.6731 0.0442 1.0000 Uiso R . . . . . .
H181 H 0.8436 0.5961 0.8177 0.0523 1.0000 Uiso R . . . . . .
H191 H 0.8388 0.5261 0.8162 0.0465 1.0000 Uiso R . . . . . .
H222 H 0.7943 0.4281 0.7292 0.0697 1.0000 Uiso R . . . . . .
H221 H 0.8502 0.4595 0.7711 0.0694 1.0000 Uiso R . . . . . .
H223 H 0.7923 0.4636 0.7977 0.0695 1.0000 Uiso R . . . . . .
H232 H 0.6074 0.6869 0.2744 0.0627 1.0000 Uiso R . . . . . .
H231 H 0.6784 0.6732 0.3199 0.0628 1.0000 Uiso R . . . . . .
H233 H 0.6401 0.6798 0.2060 0.0630 1.0000 Uiso R . . . . . .
H243 H 0.5214 0.6397 0.1771 0.0643 1.0000 Uiso R . . . . . .
H242 H 0.5527 0.6330 0.1047 0.0651 1.0000 Uiso R . . . . . .
H241 H 0.5369 0.5958 0.1561 0.0648 1.0000 Uiso R . . . . . .
H253 H 0.8266 0.5381 0.5003 0.0704 1.0000 Uiso R . . . . . .
H252 H 0.8957 0.5322 0.5873 0.0708 1.0000 Uiso R . . . . . .
H251 H 0.8833 0.5254 0.4760 0.0702 1.0000 Uiso R . . . . . .
H271 H 0.9701 0.4906 0.5589 0.0852 1.0000 Uiso R . . . . . .
H281 H 1.0472 0.4398 0.5943 0.1164 1.0000 Uiso R . . . . . .
H291 H 1.0232 0.3743 0.6172 0.1084 1.0000 Uiso R . . . . . .
H321 H 0.9503 0.3253 0.6132 0.0622 1.0000 Uiso R . . . . . .
H332 H 0.8992 0.2741 0.6114 0.0479 1.0000 Uiso R . . . . . .
H331 H 0.8230 0.2785 0.5525 0.0480 1.0000 Uiso R . . . . . .
H351 H 0.8317 0.3186 0.7721 0.0511 1.0000 Uiso R . . . . . .
H352 H 0.7853 0.2812 0.7469 0.0512 1.0000 Uiso R . . . . . .
H361 H 0.6932 0.2849 0.6179 0.0453 1.0000 Uiso R . . . . . .
H381 H 0.5866 0.2880 0.4834 0.0538 1.0000 Uiso R . . . . . .
H391 H 0.5025 0.3252 0.3691 0.0558 1.0000 Uiso R . . . . . .
H401 H 0.5168 0.3932 0.3468 0.0492 1.0000 Uiso R . . . . . .
H432 H 0.5883 0.4869 0.3769 0.0595 1.0000 Uiso R . . . . . .
H431 H 0.5593 0.4501 0.3050 0.0595 1.0000 Uiso R . . . . . .
H433 H 0.5369 0.4585 0.3886 0.0593 1.0000 Uiso R . . . . . .
H443 H 0.8377 0.2187 0.7504 0.0719 1.0000 Uiso R . . . . . .
H442 H 0.8666 0.2140 0.6738 0.0718 1.0000 Uiso R . . . . . .
H441 H 0.7947 0.2269 0.6368 0.0718 1.0000 Uiso R . . . . . .
H453 H 0.9174 0.2679 0.8531 0.0886 1.0000 Uiso R . . . . . .
H452 H 0.9360 0.3036 0.8027 0.0887 1.0000 Uiso R . . . . . .
H451 H 0.9516 0.2593 0.7856 0.0888 1.0000 Uiso R . . . . . .
H461 H 1.0728 0.3475 0.2275 0.0908 0.5000 Uiso R . . . . . .
H462 H 1.0758 0.3598 0.3263 0.0908 0.5000 Uiso R . . . . . .
H471 H 1.0494 0.4156 0.2230 0.1425 0.5000 Uiso R . . . . . .
H472 H 0.9917 0.3934 0.1483 0.1425 0.5000 Uiso R . . . . . .
H473 H 1.0000 0.4057 0.2500 0.1425 1.0000 Uiso RS . . . . . .
H481 H 0.9304 0.3418 0.1201 0.0619 0.5000 Uiso R . . . . . .
H482 H 0.9264 0.2973 0.1385 0.0619 0.5000 Uiso R . . . . . .
H491 H 0.9532 0.3044 0.0100 0.0670 0.5000 Uiso R . . . . . .
H492 H 1.0112 0.3284 0.0776 0.0670 0.5000 Uiso R . . . . . .
H493 H 1.0073 0.2839 0.0961 0.0670 0.5000 Uiso R . . . . . .
H501 H 1.0709 0.2851 0.2754 0.1119 0.5000 Uiso R . . . . . .
H502 H 1.0501 0.2851 0.3574 0.1119 0.5000 Uiso R . . . . . .
H511 H 1.0259 0.2244 0.2787 0.2680 0.5000 Uiso R . . . . . .
H512 H 0.9860 0.2457 0.1820 0.2680 0.5000 Uiso R . . . . . .
H513 H 0.9652 0.2457 0.2640 0.2680 0.5000 Uiso R . . . . . .
H521 H 0.9445 0.3614 0.2760 0.1103 0.5000 Uiso R . . . . . .
H522 H 0.9240 0.3184 0.2796 0.1103 0.5000 Uiso R . . . . . .
H531 H 0.9660 0.3539 0.4346 0.1795 0.5000 Uiso R . . . . . .
H532 H 1.0269 0.3622 0.4259 0.1795 0.5000 Uiso R . . . . . .
H533 H 1.0065 0.3192 0.4295 0.1795 0.5000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.02952(12) 0.03196(13) 0.03967(14) -0.00584(11) 0.01896(11) -0.00711(10)
Ni1 0.02700(12) 0.02085(10) 0.01911(10) 0.00045(8) 0.01049(9) 0.00175(9)
Ni2 0.03141(13) 0.02237(11) 0.03299(13) 0.00462(10) 0.01845(11) 0.00070(10)
C1 0.0331(11) 0.0286(10) 0.0471(13) -0.0089(9) 0.0232(10) -0.0018(8)
C2 0.0287(10) 0.0357(11) 0.0325(11) 0.0011(9) 0.0116(9) -0.0043(8)
C3 0.0336(11) 0.0296(10) 0.0350(11) -0.0093(8) 0.0164(9) -0.0065(8)
C4 0.086(2) 0.0222(10) 0.0475(14) -0.0012(9) 0.0425(15) 0.0033(11)
C5 0.0415(11) 0.0252(9) 0.0335(10) -0.0036(8) 0.0247(9) -0.0024(8)
C6 0.0475(13) 0.0324(11) 0.0432(13) -0.0146(9) 0.0287(11) -0.0108(10)
C7 0.0398(12) 0.0478(13) 0.0347(12) -0.0183(10) 0.0153(10) -0.0102(10)
C8 0.0389(12) 0.0458(13) 0.0259(10) -0.0084(9) 0.0109(9) -0.0009(10)
C9 0.0316(10) 0.0323(10) 0.0245(9) -0.0037(7) 0.0130(8) 0.0002(8)
C10 0.0318(10) 0.0253(8) 0.0265(9) -0.0040(7) 0.0165(8) -0.0008(7)
C11 0.0331(10) 0.0331(10) 0.0216(9) 0.0042(7) 0.0108(8) 0.0046(8)
C12 0.0320(10) 0.0277(9) 0.0253(9) 0.0044(7) 0.0142(8) 0.0002(8)
C13 0.0271(9) 0.0241(8) 0.0269(9) 0.0044(7) 0.0104(8) 0.0026(7)
C14 0.0286(10) 0.0313(10) 0.0311(10) 0.0054(8) 0.0147(8) 0.0070(8)
C15 0.0361(10) 0.0231(8) 0.0289(9) -0.0004(7) 0.0187(8) 0.0016(7)
C16 0.0320(10) 0.0280(9) 0.0243(9) -0.0029(7) 0.0140(8) -0.0005(8)
C17 0.0417(12) 0.0338(11) 0.0306(11) -0.0080(8) 0.0147(10) -0.0063(9)
C18 0.0459(14) 0.0503(14) 0.0267(11) -0.0094(10) 0.0092(10) -0.0083(11)
C19 0.0389(12) 0.0450(12) 0.0239(9) 0.0015(9) 0.0086(9) -0.0004(10)
C20 0.0314(10) 0.0317(10) 0.0244(9) 0.0012(7) 0.0117(8) 0.0016(8)
C21 0.0271(9) 0.0283(9) 0.0219(8) -0.0010(7) 0.0115(7) 0.0007(7)
C22 0.0508(15) 0.0438(13) 0.0311(11) 0.0139(10) 0.0097(11) 0.0070(11)
C23 0.0515(14) 0.0271(10) 0.0470(13) 0.0017(9) 0.0256(12) -0.0012(10)
C24 0.0338(12) 0.0507(14) 0.0337(12) 0.0044(10) 0.0063(10) 0.0051(10)
C25 0.0544(15) 0.0304(11) 0.0570(16) 0.0028(10) 0.0310(13) -0.0102(10)
C26 0.0306(11) 0.0377(12) 0.0546(15) 0.0178(11) 0.0151(11) -0.0023(9)
C27 0.0370(14) 0.0556(18) 0.105(3) 0.0360(18) 0.0233(17) -0.0054(13)
C28 0.0371(16) 0.079(3) 0.178(5) 0.064(3) 0.046(2) 0.0101(16)
C29 0.0408(17) 0.069(2) 0.168(4) 0.062(3) 0.052(2) 0.0197(15)
C30 0.0342(13) 0.0459(14) 0.090(2) 0.0319(15) 0.0308(14) 0.0093(11)
C31 0.0276(10) 0.0355(11) 0.0471(13) 0.0154(10) 0.0149(10) -0.0009(8)
C32 0.0419(14) 0.0426(14) 0.082(2) 0.0309(14) 0.0357(15) 0.0174(11)
C33 0.0493(14) 0.0280(10) 0.0448(13) 0.0059(9) 0.0264(12) 0.0101(9)
C34 0.0433(12) 0.0216(9) 0.0375(11) 0.0047(8) 0.0161(10) -0.0010(8)
C35 0.0685(17) 0.0285(10) 0.0370(12) 0.0068(9) 0.0308(12) 0.0033(11)
C36 0.0552(14) 0.0230(9) 0.0532(14) -0.0022(9) 0.0413(12) -0.0052(9)
C37 0.0437(12) 0.0307(10) 0.0463(13) -0.0060(9) 0.0325(11) -0.0075(9)
C38 0.0515(15) 0.0370(12) 0.0616(16) -0.0153(11) 0.0412(14) -0.0178(11)
C39 0.0377(13) 0.0577(16) 0.0540(15) -0.0198(12) 0.0295(12) -0.0219(12)
C40 0.0312(11) 0.0553(14) 0.0364(12) -0.0087(10) 0.0194(10) -0.0103(10)
C41 0.0320(10) 0.0376(11) 0.0301(10) -0.0066(8) 0.0192(9) -0.0064(8)
C42 0.0328(10) 0.0305(9) 0.0330(10) -0.0053(8) 0.0231(9) -0.0076(8)
C43 0.0270(10) 0.0501(14) 0.0399(12) 0.0050(10) 0.0129(9) 0.0043(10)
C44 0.0621(17) 0.0271(11) 0.0613(17) -0.0022(10) 0.0360(15) -0.0043(11)
C45 0.0583(18) 0.0532(17) 0.0494(16) 0.0104(13) 0.0108(14) -0.0099(14)
N1 0.0373(10) 0.0354(10) 0.0445(11) -0.0070(8) 0.0214(9) -0.0055(8)
N2 0.0375(10) 0.0381(10) 0.0435(11) -0.0043(9) 0.0195(9) -0.0046(8)
N3 0.0369(10) 0.0388(10) 0.0470(12) -0.0076(9) 0.0228(9) -0.0098(8)
N4 0.0309(8) 0.0258(8) 0.0236(8) 0.0019(6) 0.0143(7) 0.0021(6)
N5 0.0278(8) 0.0240(7) 0.0247(8) 0.0021(6) 0.0132(7) 0.0030(6)
N6 0.0405(10) 0.0296(9) 0.0445(11) 0.0134(8) 0.0233(9) 0.0079(8)
N7 0.0487(11) 0.0239(8) 0.0389(10) 0.0038(7) 0.0295(9) 0.0019(7)
O1 0.0617(11) 0.0213(7) 0.0352(8) -0.0014(6) 0.0278(8) 0.0028(7)
O2 0.0373(8) 0.0232(6) 0.0220(6) -0.0011(5) 0.0118(6) 0.0016(6)
O3 0.0382(8) 0.0229(6) 0.0208(6) -0.0001(5) 0.0112(6) 0.0005(6)
O4 0.0453(9) 0.0319(8) 0.0246(7) 0.0066(6) 0.0116(7) 0.0045(7)
O5 0.0367(9) 0.0282(8) 0.0569(11) 0.0091(7) 0.0241(8) -0.0033(6)
O6 0.0263(7) 0.0267(7) 0.0428(9) 0.0081(6) 0.0161(7) 0.0011(5)
O7 0.0302(7) 0.0245(7) 0.0346(8) 0.0006(6) 0.0175(6) -0.0023(5)
O8 0.0276(7) 0.0364(8) 0.0351(8) 0.0013(6) 0.0127(6) -0.0014(6)
S1 0.0553(4) 0.0429(3) 0.0448(3) 0.0017(3) 0.0243(3) 0.0081(3)
S2 0.0439(3) 0.0344(3) 0.0523(4) -0.0018(3) 0.0186(3) 0.0041(2)
S3 0.0475(4) 0.0472(4) 0.0636(4) -0.0143(3) 0.0369(3) -0.0208(3)
Na1 0.0304(4) 0.0230(4) 0.0314(4) 0.0030(3) 0.0138(3) 0.0008(3)
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 . N2 4_666 2.109(2) yes
Mo1 . N1 4_666 2.104(2) yes
Mo1 . N3 4_666 2.0905(19) yes
Mo1 . N1 . 2.104(2) yes
Mo1 . N2 . 2.109(2) yes
Mo1 . N3 . 2.0905(19) yes
Ni1 . N4 . 1.8614(17) yes
Ni1 . N5 . 1.8667(16) yes
Ni1 . O2 . 1.8522(14) yes
Ni1 . O3 . 1.8443(14) yes
Ni2 . N6 . 1.868(2) yes
Ni2 . N7 . 1.8626(18) yes
Ni2 . O6 . 1.8467(14) yes
Ni2 . O7 . 1.8655(15) yes
C1 . N1 . 1.163(3) yes
C1 . S1 . 1.630(3) yes
C2 . N2 . 1.166(3) yes
C2 . S2 . 1.623(2) yes
C3 . N3 . 1.155(3) yes
C3 . S3 . 1.616(2) yes
C4 . O1 . 1.431(3) yes
C4 . H43 . 0.972 no
C4 . H42 . 0.964 no
C4 . H41 . 0.975 no
C5 . C6 . 1.381(3) yes
C5 . C10 . 1.423(3) yes
C5 . O1 . 1.368(3) yes
C6 . C7 . 1.395(4) yes
C6 . H61 . 0.944 no
C7 . C8 . 1.364(4) yes
C7 . H71 . 0.937 no
C8 . C9 . 1.413(3) yes
C8 . H81 . 0.943 no
C9 . C10 . 1.405(3) yes
C9 . C11 . 1.435(3) yes
C10 . O2 . 1.317(2) yes
C11 . N4 . 1.290(3) yes
C11 . H111 . 0.949 no
C12 . C13 . 1.530(3) yes
C12 . N4 . 1.472(3) yes
C12 . H122 . 0.974 no
C12 . H121 . 0.979 no
C13 . C14 . 1.535(3) yes
C13 . C23 . 1.526(3) yes
C13 . C24 . 1.528(3) yes
C14 . N5 . 1.475(3) yes
C14 . H141 . 0.975 no
C14 . H142 . 0.984 no
C15 . C16 . 1.433(3) yes
C15 . N5 . 1.292(3) yes
C15 . H151 . 0.961 no
C16 . C17 . 1.413(3) yes
C16 . C21 . 1.404(3) yes
C17 . C18 . 1.367(4) yes
C17 . H171 . 0.943 no
C18 . C19 . 1.403(4) yes
C18 . H181 . 0.946 no
C19 . C20 . 1.376(3) yes
C19 . H191 . 0.947 no
C20 . C21 . 1.424(3) yes
C20 . O4 . 1.368(3) yes
C21 . O3 . 1.317(2) yes
C22 . O4 . 1.422(3) yes
C22 . H222 . 0.963 no
C22 . H221 . 0.966 no
C22 . H223 . 0.968 no
C23 . H232 . 0.957 no
C23 . H231 . 0.960 no
C23 . H233 . 0.956 no
C24 . H243 . 0.962 no
C24 . H242 . 0.962 no
C24 . H241 . 0.964 no
C25 . O5 . 1.425(3) yes
C25 . H253 . 0.970 no
C25 . H252 . 0.958 no
C25 . H251 . 0.976 no
C26 . C27 . 1.374(4) yes
C26 . C31 . 1.427(3) yes
C26 . O5 . 1.366(3) yes
C27 . C28 . 1.412(5) yes
C27 . H271 . 0.948 no
C28 . C29 . 1.357(5) yes
C28 . H281 . 0.956 no
C29 . C30 . 1.419(4) yes
C29 . H291 . 0.955 no
C30 . C31 . 1.409(4) yes
C30 . C32 . 1.426(4) yes
C31 . O6 . 1.305(3) yes
C32 . N6 . 1.284(3) yes
C32 . H321 . 0.956 no
C33 . C34 . 1.533(3) yes
C33 . N6 . 1.470(3) yes
C33 . H332 . 0.981 no
C33 . H331 . 0.998 no
C34 . C35 . 1.534(4) yes
C34 . C44 . 1.523(3) yes
C34 . C45 . 1.529(4) yes
C35 . N7 . 1.472(3) yes
C35 . H351 . 0.979 no
C35 . H352 . 0.963 no
C36 . C37 . 1.437(4) yes
C36 . N7 . 1.291(3) yes
C36 . H361 . 0.957 no
C37 . C38 . 1.414(3) yes
C37 . C42 . 1.413(3) yes
C38 . C39 . 1.355(4) yes
C38 . H381 . 0.942 no
C39 . C40 . 1.402(4) yes
C39 . H391 . 0.951 no
C40 . C41 . 1.384(3) yes
C40 . H401 . 0.953 no
C41 . C42 . 1.421(3) yes
C41 . O8 . 1.368(3) yes
C42 . O7 . 1.315(2) yes
C43 . O8 . 1.428(3) yes
C43 . H432 . 0.967 no
C43 . H431 . 0.965 no
C43 . H433 . 0.979 no
C44 . H443 . 0.969 no
C44 . H442 . 0.968 no
C44 . H441 . 0.964 no
C45 . H453 . 0.959 no
C45 . H452 . 0.961 no
C45 . H451 . 0.962 no
O1 . Na1 . 2.5581(18) yes
O2 . Na1 . 2.3573(16) yes
O3 . Na1 . 2.3551(16) yes
O4 . Na1 . 2.5116(18) yes
O5 . Na1 . 2.5958(18) yes
O6 . Na1 . 2.3573(17) yes
O7 . Na1 . 2.3851(16) yes
O8 . Na1 . 2.5593(17) yes
N8 . C46 5_755 1.547(9) yes
N8 . C52 5_755 1.510(9) yes
N8 . C48 5_755 1.509(6) yes
N8 . C50 5_755 1.486(9) yes
N8 . C46 . 1.547(9) yes
N8 . C48 . 1.509(6) yes
N8 . C50 . 1.486(9) yes
N8 . C52 . 1.510(9) yes
C46 . C47 . 1.546(12) yes
C46 . H461 . 0.930 no
C46 . H462 . 0.930 no
C47 . H471 . 0.930 no
C47 . H472 . 0.930 no
C47 . H473 . 0.866 no
C48 . C49 . 1.530(9) yes
C48 . H481 . 0.930 no
C48 . H482 . 0.930 no
C49 . H491 . 0.930 no
C49 . H492 . 0.930 no
C49 . H493 . 0.930 no
C50 . C50 5_755 1.582(19) yes
C50 . C51 . 1.519(13) yes
C50 . H501 . 0.930 no
C50 . H502 . 0.930 no
C51 . H511 5_755 0.930 no
C51 . H512 5_755 0.930 no
C51 . H513 5_755 0.930 no
C51 . H511 . 0.930 no
C51 . H512 . 0.930 no
C51 . H513 . 0.930 no
C52 . C53 . 1.507(19) yes
C52 . H521 . 0.930 no
C52 . H522 . 0.930 no
C53 . H492 5_755 0.619 no
C53 . H531 . 0.930 no
C53 . H532 . 0.930 no
C53 . H533 . 0.930 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 4_666 Mo1 . N1 4_666 88.49(8) yes
N2 4_666 Mo1 . N3 4_666 92.20(8) yes
N1 4_666 Mo1 . N3 4_666 87.24(8) yes
N2 4_666 Mo1 . N1 . 91.51(8) yes
N1 4_666 Mo1 . N1 . 179.995 yes
N3 4_666 Mo1 . N1 . 92.76(8) yes
N2 4_666 Mo1 . N2 . 179.995 yes
N1 4_666 Mo1 . N2 . 91.51(8) yes
N3 4_666 Mo1 . N2 . 87.80(8) yes
N1 . Mo1 . N2 . 88.49(8) yes
N2 4_666 Mo1 . N3 . 87.80(8) yes
N1 4_666 Mo1 . N3 . 92.76(8) yes
N3 4_666 Mo1 . N3 . 179.995 yes
N1 . Mo1 . N3 . 87.24(8) yes
N2 . Mo1 . N3 . 92.20(8) yes
N4 . Ni1 . N5 . 91.33(7) yes
N4 . Ni1 . O2 . 92.26(7) yes
N5 . Ni1 . O2 . 175.49(7) yes
N4 . Ni1 . O3 . 176.32(7) yes
N5 . Ni1 . O3 . 91.72(7) yes
O2 . Ni1 . O3 . 84.80(6) yes
N6 . Ni2 . N7 . 90.86(8) yes
N6 . Ni2 . O6 . 94.22(8) yes
N7 . Ni2 . O6 . 171.63(8) yes
N6 . Ni2 . O7 . 170.32(8) yes
N7 . Ni2 . O7 . 91.37(8) yes
O6 . Ni2 . O7 . 84.73(6) yes
N1 . C1 . S1 . 179.6(2) yes
N2 . C2 . S2 . 179.1(2) yes
N3 . C3 . S3 . 179.0(2) yes
O1 . C4 . H43 . 108.3 no
O1 . C4 . H42 . 108.7 no
H43 . C4 . H42 . 109.0 no
O1 . C4 . H41 . 109.6 no
H43 . C4 . H41 . 112.1 no
H42 . C4 . H41 . 109.0 no
C6 . C5 . C10 . 120.7(2) yes
C6 . C5 . O1 . 125.1(2) yes
C10 . C5 . O1 . 114.19(19) yes
C5 . C6 . C7 . 120.4(2) yes
C5 . C6 . H61 . 120.2 no
C7 . C6 . H61 . 119.4 no
C6 . C7 . C8 . 120.3(2) yes
C6 . C7 . H71 . 119.2 no
C8 . C7 . H71 . 120.6 no
C7 . C8 . C9 . 120.3(2) yes
C7 . C8 . H81 . 120.3 no
C9 . C8 . H81 . 119.3 no
C8 . C9 . C10 . 120.5(2) yes
C8 . C9 . C11 . 119.9(2) yes
C10 . C9 . C11 . 119.45(19) yes
C5 . C10 . C9 . 117.53(19) yes
C5 . C10 . O2 . 118.67(19) yes
C9 . C10 . O2 . 123.79(18) yes
C9 . C11 . N4 . 124.97(19) yes
C9 . C11 . H111 . 117.6 no
N4 . C11 . H111 . 117.4 no
C13 . C12 . N4 . 111.55(16) yes
C13 . C12 . H122 . 108.7 no
N4 . C12 . H122 . 108.5 no
C13 . C12 . H121 . 109.4 no
N4 . C12 . H121 . 109.2 no
H122 . C12 . H121 . 109.5 no
C12 . C13 . C14 . 110.09(16) yes
C12 . C13 . C23 . 108.48(18) yes
C14 . C13 . C23 . 110.05(18) yes
C12 . C13 . C24 . 110.00(18) yes
C14 . C13 . C24 . 108.62(18) yes
C23 . C13 . C24 . 109.59(19) yes
C13 . C14 . N5 . 114.17(16) yes
C13 . C14 . H141 . 108.9 no
N5 . C14 . H141 . 109.1 no
C13 . C14 . H142 . 108.8 no
N5 . C14 . H142 . 106.7 no
H141 . C14 . H142 . 109.0 no
C16 . C15 . N5 . 124.57(18) yes
C16 . C15 . H151 . 117.8 no
N5 . C15 . H151 . 117.5 no
C15 . C16 . C17 . 120.05(19) yes
C15 . C16 . C21 . 119.02(18) yes
C17 . C16 . C21 . 120.0(2) yes
C16 . C17 . C18 . 120.4(2) yes
C16 . C17 . H171 . 118.2 no
C18 . C17 . H171 . 121.3 no
C17 . C18 . C19 . 120.1(2) yes
C17 . C18 . H181 . 120.9 no
C19 . C18 . H181 . 118.9 no
C18 . C19 . C20 . 120.5(2) yes
C18 . C19 . H191 . 119.8 no
C20 . C19 . H191 . 119.7 no
C19 . C20 . C21 . 120.4(2) yes
C19 . C20 . O4 . 126.2(2) yes
C21 . C20 . O4 . 113.40(18) yes
C20 . C21 . C16 . 118.29(18) yes
C20 . C21 . O3 . 117.60(18) yes
C16 . C21 . O3 . 124.10(18) yes
O4 . C22 . H222 . 107.6 no
O4 . C22 . H221 . 108.7 no
H222 . C22 . H221 . 109.6 no
O4 . C22 . H223 . 110.5 no
H222 . C22 . H223 . 110.4 no
H221 . C22 . H223 . 109.9 no
C13 . C23 . H232 . 109.3 no
C13 . C23 . H231 . 110.2 no
H232 . C23 . H231 . 109.4 no
C13 . C23 . H233 . 109.7 no
H232 . C23 . H233 . 108.7 no
H231 . C23 . H233 . 109.5 no
C13 . C24 . H243 . 107.7 no
C13 . C24 . H242 . 109.1 no
H243 . C24 . H242 . 110.5 no
C13 . C24 . H241 . 108.8 no
H243 . C24 . H241 . 109.4 no
H242 . C24 . H241 . 111.2 no
O5 . C25 . H253 . 107.7 no
O5 . C25 . H252 . 109.1 no
H253 . C25 . H252 . 110.6 no
O5 . C25 . H251 . 109.1 no
H253 . C25 . H251 . 109.6 no
H252 . C25 . H251 . 110.8 no
C27 . C26 . C31 . 120.2(2) yes
C27 . C26 . O5 . 125.4(2) yes
C31 . C26 . O5 . 114.4(2) yes
C26 . C27 . C28 . 121.1(3) yes
C26 . C27 . H271 . 119.3 no
C28 . C27 . H271 . 119.6 no
C27 . C28 . C29 . 120.0(3) yes
C27 . C28 . H281 . 120.1 no
C29 . C28 . H281 . 119.9 no
C28 . C29 . C30 . 120.2(3) yes
C28 . C29 . H291 . 120.5 no
C30 . C29 . H291 . 119.3 no
C29 . C30 . C31 . 120.6(3) yes
C29 . C30 . C32 . 118.6(3) yes
C31 . C30 . C32 . 120.8(2) yes
C26 . C31 . C30 . 117.9(2) yes
C26 . C31 . O6 . 118.2(2) yes
C30 . C31 . O6 . 123.9(2) yes
C30 . C32 . N6 . 126.4(2) yes
C30 . C32 . H321 . 115.9 no
N6 . C32 . H321 . 117.8 no
C34 . C33 . N6 . 112.79(19) yes
C34 . C33 . H332 . 107.6 no
N6 . C33 . H332 . 109.8 no
C34 . C33 . H331 . 109.6 no
N6 . C33 . H331 . 107.8 no
H332 . C33 . H331 . 109.2 no
C33 . C34 . C35 . 110.40(18) yes
C33 . C34 . C44 . 107.4(2) yes
C35 . C34 . C44 . 110.2(2) yes
C33 . C34 . C45 . 110.6(2) yes
C35 . C34 . C45 . 109.0(2) yes
C44 . C34 . C45 . 109.1(2) yes
C34 . C35 . N7 . 113.02(18) yes
C34 . C35 . H351 . 108.1 no
N7 . C35 . H351 . 107.2 no
C34 . C35 . H352 . 109.8 no
N7 . C35 . H352 . 108.9 no
H351 . C35 . H352 . 109.8 no
C37 . C36 . N7 . 124.6(2) yes
C37 . C36 . H361 . 117.7 no
N7 . C36 . H361 . 117.7 no
C36 . C37 . C38 . 120.2(2) yes
C36 . C37 . C42 . 119.2(2) yes
C38 . C37 . C42 . 120.2(2) yes
C37 . C38 . C39 . 121.0(2) yes
C37 . C38 . H381 . 118.3 no
C39 . C38 . H381 . 120.7 no
C38 . C39 . C40 . 119.9(2) yes
C38 . C39 . H391 . 120.8 no
C40 . C39 . H391 . 119.2 no
C39 . C40 . C41 . 120.4(3) yes
C39 . C40 . H401 . 119.4 no
C41 . C40 . H401 . 120.3 no
C40 . C41 . C42 . 120.8(2) yes
C40 . C41 . O8 . 124.8(2) yes
C42 . C41 . O8 . 114.32(18) yes
C41 . C42 . C37 . 117.4(2) yes
C41 . C42 . O7 . 118.79(19) yes
C37 . C42 . O7 . 123.8(2) yes
O8 . C43 . H432 . 107.6 no
O8 . C43 . H431 . 109.2 no
H432 . C43 . H431 . 109.4 no
O8 . C43 . H433 . 109.6 no
H432 . C43 . H433 . 111.1 no
H431 . C43 . H433 . 110.0 no
C34 . C44 . H443 . 108.6 no
C34 . C44 . H442 . 108.7 no
H443 . C44 . H442 . 109.9 no
C34 . C44 . H441 . 109.3 no
H443 . C44 . H441 . 110.0 no
H442 . C44 . H441 . 110.2 no
C34 . C45 . H453 . 108.9 no
C34 . C45 . H452 . 109.1 no
H453 . C45 . H452 . 110.2 no
C34 . C45 . H451 . 108.6 no
H453 . C45 . H451 . 110.7 no
H452 . C45 . H451 . 109.4 no
Mo1 . N1 . C1 . 172.33(19) yes
Mo1 . N2 . C2 . 176.66(19) yes
Mo1 . N3 . C3 . 168.8(2) yes
C12 . N4 . C11 . 118.45(17) yes
C12 . N4 . Ni1 . 116.27(13) yes
C11 . N4 . Ni1 . 125.25(15) yes
C14 . N5 . C15 . 118.44(17) yes
C14 . N5 . Ni1 . 116.52(13) yes
C15 . N5 . Ni1 . 124.72(14) yes
C33 . N6 . C32 . 116.4(2) yes
C33 . N6 . Ni2 . 117.29(16) yes
C32 . N6 . Ni2 . 125.72(17) yes
C35 . N7 . C36 . 119.2(2) yes
C35 . N7 . Ni2 . 116.43(16) yes
C36 . N7 . Ni2 . 124.27(17) yes
C4 . O1 . C5 . 116.10(19) yes
C4 . O1 . Na1 . 126.44(15) yes
C5 . O1 . Na1 . 115.72(12) yes
C10 . O2 . Ni1 . 124.51(13) yes
C10 . O2 . Na1 . 122.99(12) yes
Ni1 . O2 . Na1 . 105.48(6) yes
C21 . O3 . Ni1 . 124.62(13) yes
C21 . O3 . Na1 . 121.63(12) yes
Ni1 . O3 . Na1 . 105.83(6) yes
C22 . O4 . C20 . 117.19(19) yes
C22 . O4 . Na1 . 122.96(15) yes
C20 . O4 . Na1 . 115.83(12) yes
C25 . O5 . C26 . 116.84(19) yes
C25 . O5 . Na1 . 126.38(15) yes
C26 . O5 . Na1 . 116.69(13) yes
C31 . O6 . Ni2 . 127.64(14) yes
C31 . O6 . Na1 . 125.81(13) yes
Ni2 . O6 . Na1 . 106.53(7) yes
C42 . O7 . Ni2 . 121.95(13) yes
C42 . O7 . Na1 . 121.33(13) yes
Ni2 . O7 . Na1 . 104.82(6) yes
C43 . O8 . C41 . 117.00(18) yes
C43 . O8 . Na1 . 122.51(14) yes
C41 . O8 . Na1 . 115.08(13) yes
O3 . Na1 . O2 . 63.87(5) yes
O3 . Na1 . O6 . 140.25(7) yes
O2 . Na1 . O6 . 132.22(6) yes
O3 . Na1 . O7 . 135.50(6) yes
O2 . Na1 . O7 . 136.62(6) yes
O6 . Na1 . O7 . 63.67(5) yes
O3 . Na1 . O4 . 63.93(5) yes
O2 . Na1 . O4 . 127.47(6) yes
O6 . Na1 . O4 . 87.52(6) yes
O7 . Na1 . O4 . 87.32(6) yes
O3 . Na1 . O1 . 126.56(6) yes
O2 . Na1 . O1 . 64.24(5) yes
O6 . Na1 . O1 . 86.42(6) yes
O7 . Na1 . O1 . 79.80(6) yes
O4 . Na1 . O1 . 167.12(6) yes
O3 . Na1 . O8 . 87.91(6) yes
O2 . Na1 . O8 . 82.50(6) yes
O6 . Na1 . O8 . 126.26(6) yes
O7 . Na1 . O8 . 63.91(5) yes
O4 . Na1 . O8 . 101.08(6) yes
O3 . Na1 . O5 . 83.33(6) yes
O2 . Na1 . O5 . 89.98(6) yes
O6 . Na1 . O5 . 63.39(5) yes
O7 . Na1 . O5 . 125.56(6) yes
O4 . Na1 . O5 . 78.69(6) yes
O1 . Na1 . O8 . 73.65(6) yes
O1 . Na1 . O5 . 108.51(7) yes
O8 . Na1 . O5 . 170.34(6) yes
C46 5_755 N8 . C52 5_755 112.0(6) yes
C46 5_755 N8 . C48 5_755 109.4(4) yes
C52 5_755 N8 . C48 5_755 103.8(4) yes
C46 5_755 N8 . C50 5_755 106.9(5) yes
C52 5_755 N8 . C50 5_755 114.4(6) yes
C48 5_755 N8 . C50 5_755 110.5(5) yes
C46 5_755 N8 . C46 . 90.3(7) yes
C48 5_755 N8 . C46 . 79.8(4) yes
C50 5_755 N8 . C46 . 154.7(5) yes
C46 5_755 N8 . C48 . 79.8(4) yes
C52 5_755 N8 . C48 . 79.7(4) yes
C48 5_755 N8 . C48 . 167.5(6) yes
C50 5_755 N8 . C48 . 57.7(4) yes
C46 . N8 . C48 . 109.4(4) yes
C46 5_755 N8 . C50 . 154.7(5) yes
C52 5_755 N8 . C50 . 92.9(5) yes
C48 5_755 N8 . C50 . 57.7(4) yes
C50 5_755 N8 . C50 . 64.3(8) yes
C46 . N8 . C50 . 106.9(5) yes
C52 5_755 N8 . C52 . 148.2(8) yes
C48 5_755 N8 . C52 . 79.7(4) yes
C50 5_755 N8 . C52 . 92.9(5) yes
C46 . N8 . C52 . 112.0(6) yes
C48 . N8 . C50 . 110.5(5) yes
C48 . N8 . C52 . 103.8(4) yes
C50 . N8 . C52 . 114.4(6) yes
N8 . C46 . C47 . 113.2(6) yes
N8 . C46 . H461 . 109.3 no
C47 . C46 . H461 . 108.2 no
N8 . C46 . H462 . 108.5 no
C47 . C46 . H462 . 108.1 no
H461 . C46 . H462 . 109.5 no
C46 . C47 . H471 . 110.4 no
C46 . C47 . H472 . 109.0 no
H471 . C47 . H472 . 109.5 no
C46 . C47 . H473 . 107.4 no
H471 . C47 . H473 . 105.3 no
H472 . C47 . H473 . 115.2 no
N8 . C48 . C49 . 114.6(5) yes
N8 . C48 . H481 . 109.2 no
C49 . C48 . H481 . 108.9 no
N8 . C48 . H482 . 107.6 no
C49 . C48 . H482 . 106.9 no
H481 . C48 . H482 . 109.5 no
C48 . C49 . H491 . 110.6 no
C48 . C49 . H492 . 107.9 no
H491 . C49 . H492 . 109.5 no
C48 . C49 . H493 . 109.9 no
H491 . C49 . H493 . 109.5 no
H492 . C49 . H493 . 109.5 no
C50 5_755 C50 . N8 . 57.8(4) yes
C50 5_755 C50 . C51 . 58.6(5) yes
N8 . C50 . C51 . 116.5(7) yes
C50 5_755 C50 . H501 . 125.9 no
N8 . C50 . H501 . 108.8 no
C51 . C50 . H501 . 107.1 no
C50 5_755 C50 . H502 . 124.7 no
N8 . C50 . H502 . 108.2 no
C51 . C50 . H502 . 106.6 no
H501 . C50 . H502 . 109.5 no
C50 5_755 C51 . C50 . 62.8(9) yes
C50 5_755 C51 . H511 5_755 110.8 no
C50 . C51 . H511 5_755 173.6 no
C50 5_755 C51 . H512 5_755 108.5 no
C50 . C51 . H512 5_755 74.1 no
H511 5_755 C51 . H512 5_755 109.5 no
C50 5_755 C51 . H513 5_755 109.0 no
C50 . C51 . H513 5_755 73.5 no
H511 5_755 C51 . H513 5_755 109.5 no
H512 5_755 C51 . H513 5_755 109.5 no
C50 5_755 C51 . H511 . 173.6 no
C50 . C51 . H511 . 110.8 no
H511 5_755 C51 . H511 . 75.6 no
H512 5_755 C51 . H511 . 68.1 no
H513 5_755 C51 . H511 . 68.1 no
C50 5_755 C51 . H512 . 74.1 no
C50 . C51 . H512 . 108.5 no
H511 5_755 C51 . H512 . 68.1 no
H512 5_755 C51 . H512 . 177.1 no
H513 5_755 C51 . H512 . 70.4 no
C50 5_755 C51 . H513 . 73.5 no
C50 . C51 . H513 . 109.0 no
H511 5_755 C51 . H513 . 68.1 no
H512 5_755 C51 . H513 . 70.4 no
H513 5_755 C51 . H513 . 177.1 no
H511 . C51 . H512 . 109.5 no
H511 . C51 . H513 . 109.5 no
H512 . C51 . H513 . 109.5 no
N8 . C52 . C53 . 116.5(10) yes
N8 . C52 . H521 . 106.2 no
C53 . C52 . H521 . 97.8 no
N8 . C52 . H522 . 110.2 no
C53 . C52 . H522 . 115.4 no
H521 . C52 . H522 . 109.5 no
C52 . C53 . H492 5_755 97.2 no
C52 . C53 . H531 . 114.8 no
H492 5_755 C53 . H531 . 84.0 no
C52 . C53 . H532 . 115.2 no
H492 5_755 C53 . H532 . 132.8 no
H531 . C53 . H532 . 109.5 no
C52 . C53 . H533 . 97.6 no
H531 . C53 . H533 . 109.5 no
H532 . C53 . H533 . 109.5 no
C47 5_755 H473 . C47 . 139.9 no
C49 . H492 . C53 5_755 119.1 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C12 . H121 . C42 6_564 169 0.98 2.60 3.565(5) yes
C47 . H473 . C47 5_755 140 0.87 0.87 1.628(5) yes
C50 . H502 . C49 5_755 128 0.93 1.73 2.417(5) yes
C48 5_755 H502 . C51 . 129 1.11 1.99 2.822(5) yes
C52 . H521 . C47 5_755 128 0.93 1.44 2.141(5) yes
# Attachment '- 4_new_ccdc809270.cif'
data_4
_database_code_depnum_ccdc_archive 'CCDC 809270'
#TrackingRef '- 4_new_ccdc809270.cif'
_audit_creation_date 11-04-19
_audit_creation_method CRYSTALS_ver_14.09
_oxford_structure_analysis_title 'JPS0941_111209_0m in Pnma'
_chemical_name_systematic ?
_chemical_melting_point ?
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 7.4030(5)
_cell_length_b 16.4860(10)
_cell_length_c 18.0343(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 2201.0(2)
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P n m a '
_symmetry_space_group_name_Hall '-P 2ac 2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_sum 'C22 H24 Cu1 K1 N3 O4 S1'
_chemical_formula_moiety 'C22 H24 Cu1 K1 N3 O4 S1'
_chemical_compound_source ?
_chemical_formula_weight 529.16
_cell_measurement_reflns_used 7116
_cell_measurement_theta_min 3
_cell_measurement_theta_max 35
_cell_measurement_temperature 180
_exptl_crystal_description stick
_exptl_crystal_colour green
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.150
_exptl_crystal_size_max 0.300
_exptl_crystal_density_diffrn 1.597
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1092
_exptl_absorpt_coefficient_mu 1.312
# Sheldrick geometric approximatio 0.82 0.88
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min 0.82
_exptl_absorpt_correction_T_max 0.88
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 180
_diffrn_reflns_number 19159
_reflns_number_total 4812
_diffrn_reflns_av_R_equivalents 0.031
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 4812
# Theoretical number of reflections is about 9933
_diffrn_reflns_theta_min 2.259
_diffrn_reflns_theta_max 35.331
_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full 33.565
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 28
_reflns_limit_h_min 0
_reflns_limit_h_max 12
_reflns_limit_k_min 0
_reflns_limit_k_max 25
_reflns_limit_l_min 0
_reflns_limit_l_max 28
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.55
_refine_diff_density_max 0.60
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 3623
_refine_ls_number_restraints 4
_refine_ls_number_parameters 159
_oxford_refine_ls_R_factor_ref 0.0292
_refine_ls_wR_factor_ref 0.0373
_refine_ls_goodness_of_fit_ref 1.0364
_refine_ls_shift/su_max 0.0292972
_refine_ls_shift/su_mean 0.0002757
# The values computed from all data
_oxford_reflns_number_all 4803
_refine_ls_R_factor_all 0.0450
_refine_ls_wR_factor_all 0.0459
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 3857
_refine_ls_R_factor_gt 0.0317
_refine_ls_wR_factor_gt 0.0385
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.921 0.653 0.627
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O1 O 0.66986(17) 0.59615(6) 0.22567(5) 0.0294 1.0000 Uani . . . . . .
O2 O 0.74489(14) 0.67332(5) 0.34704(5) 0.0184 1.0000 Uani . . . . . .
C1 C 0.6593(2) 0.55218(10) 0.15763(8) 0.0330 1.0000 Uani . . . . . .
C2 C 0.66027(18) 0.55156(8) 0.28956(7) 0.0212 1.0000 Uani . . . . . .
C3 C 0.6156(2) 0.47041(8) 0.29361(9) 0.0277 1.0000 Uani . . . . . .
C4 C 0.6123(2) 0.43036(8) 0.36248(9) 0.0294 1.0000 Uani . . . . . .
C5 C 0.65819(19) 0.47138(8) 0.42580(8) 0.0238 1.0000 Uani . . . . . .
C6 C 0.70744(16) 0.55449(7) 0.42278(6) 0.0177 1.0000 Uani . . . . . .
C7 C 0.70442(16) 0.59696(7) 0.35475(6) 0.0161 1.0000 Uani . . . . . .
C8 C 0.78835(16) 0.58880(7) 0.48816(6) 0.0180 1.0000 Uani . . . . . .
C9 C 0.96469(18) 0.67388(8) 0.56281(6) 0.0200 1.0000 Uani . . . . . .
C10 C 0.9249(2) 0.7500 0.60811(8) 0.0192 1.0000 Uani S T . . . .
C11 C 0.7320(3) 0.750000(7) 0.63810(11) 0.0296 1.0000 Uani S T . . . .
C12 C 1.0583(3) 0.750000(7) 0.67310(11) 0.0307 1.0000 Uani S T . . . .
C13 C 1.2622(3) 0.7500 0.42162(10) 0.0226 1.0000 Uani S T . . . .
Cu1 Cu 0.80138(3) 0.7500 0.424988(10) 0.0149 1.0000 Uani S T . . . .
K1 K 0.46198(5) 0.7500 0.259990(19) 0.0211 1.0000 Uani S T . . . .
S1 S 1.42240(7) 0.7500 0.48409(3) 0.0385 1.0000 Uani S T . . . .
N1 N 0.85042(14) 0.66147(6) 0.49709(5) 0.0158 1.0000 Uani . . . . . .
N2 N 1.1469(3) 0.7500 0.37773(11) 0.0352 1.0000 Uani S T . . . .
H11 H 0.5436 0.5257 0.1540 0.0526 1.0000 Uiso R . . . . .
H12 H 0.7528 0.5120 0.1560 0.0525 1.0000 Uiso R . . . . .
H13 H 0.6729 0.5919 0.1179 0.0525 1.0000 Uiso R . . . . .
H31 H 0.5896 0.4401 0.2504 0.0353 1.0000 Uiso R . . . . .
H41 H 0.5803 0.3731 0.3644 0.0372 1.0000 Uiso R . . . . .
H51 H 0.6599 0.4448 0.4719 0.0312 1.0000 Uiso R . . . . .
H81 H 0.8031 0.5518 0.5273 0.0243 1.0000 Uiso R . . . . .
H91 H 1.0909 0.6730 0.5469 0.0262 1.0000 Uiso R . . . . .
H92 H 0.9462 0.6294 0.5971 0.0261 1.0000 Uiso R . . . . .
H111 H 0.7041 0.7040 0.6687 0.0500 1.0000 Uiso R . . . . .
H112 H 0.6549 0.7500 0.5969 0.0500 1.0000 Uiso RS . . . . .
H121 H 1.1775 0.7500 0.6551 0.0396 1.0000 Uiso RS . . . . .
H122 H 1.0396 0.7034 0.7022 0.0396 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0481(6) 0.0238(4) 0.0163(4) -0.0066(3) -0.0085(4) 0.0051(4)
O2 0.0282(4) 0.0138(3) 0.0132(3) -0.0009(3) -0.0027(3) -0.0018(3)
C1 0.0427(8) 0.0350(7) 0.0212(5) -0.0152(5) -0.0112(5) 0.0112(6)
C2 0.0234(5) 0.0184(5) 0.0218(5) -0.0061(4) -0.0057(4) 0.0037(4)
C3 0.0300(6) 0.0186(5) 0.0345(7) -0.0098(5) -0.0083(5) 0.0009(5)
C4 0.0303(7) 0.0159(5) 0.0421(7) -0.0046(5) -0.0040(6) -0.0026(5)
C5 0.0252(5) 0.0157(4) 0.0306(6) 0.0015(4) 0.0013(5) -0.0019(4)
C6 0.0194(5) 0.0142(4) 0.0195(4) 0.0000(3) 0.0007(4) 0.0001(3)
C7 0.0174(4) 0.0145(4) 0.0163(4) -0.0020(3) -0.0009(3) 0.0010(4)
C8 0.0215(5) 0.0165(4) 0.0161(4) 0.0031(3) 0.0010(4) 0.0011(4)
C9 0.0229(5) 0.0222(5) 0.0149(4) 0.0021(4) -0.0053(4) 0.0018(4)
C10 0.0195(7) 0.0272(8) 0.0109(5) 0.0000 -0.0029(5) 0.0000
C11 0.0224(8) 0.0501(12) 0.0164(7) 0.0000 0.0041(6) 0.0000
C12 0.0355(11) 0.0379(10) 0.0188(7) 0.0000 -0.0130(7) 0.0000
C13 0.0217(7) 0.0282(8) 0.0180(7) 0.0000 0.0028(6) 0.0000
Cu1 0.02240(10) 0.01235(8) 0.00984(8) 0.0000 -0.00287(6) 0.0000
K1 0.01843(15) 0.02898(17) 0.01577(14) 0.0000 -0.00087(11) 0.0000
S1 0.0177(2) 0.0724(4) 0.0255(2) 0.0000 -0.00314(17) 0.0000
N1 0.0183(4) 0.0176(4) 0.0116(3) 0.0013(3) -0.0008(3) 0.0006(3)
N2 0.0359(10) 0.0446(11) 0.0251(8) 0.0000 -0.0058(7) 0.0000
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C1 . 1.4272(16) yes
O1 . C2 . 1.3685(17) yes
O2 . C7 . 1.3015(14) yes
O2 . Cu1 . 1.9363(8) yes
C1 . H11 . 0.963 no
C1 . H12 . 0.959 no
C1 . H13 . 0.976 no
C2 . C3 . 1.3800(19) yes
C2 . C7 . 1.4315(16) yes
C3 . C4 . 1.407(2) yes
C3 . H31 . 0.946 no
C4 . C5 . 1.370(2) yes
C4 . H41 . 0.974 no
C5 . C6 . 1.4188(17) yes
C5 . H51 . 0.939 no
C6 . C7 . 1.4128(16) yes
C6 . C8 . 1.4384(17) yes
C8 . N1 . 1.2932(15) yes
C8 . H81 . 0.939 no
C9 . C10 . 1.5261(15) yes
C9 . N1 . 1.4705(15) yes
C9 . H91 . 0.978 no
C9 . H92 . 0.969 no
C10 . C11 . 1.527(3) yes
C10 . C12 . 1.533(2) yes
C11 . H111 5_565 0.960 no
C11 . H111 . 0.960 no
C11 . H112 . 0.937 no
C12 . H122 5_565 0.940 no
C12 . H121 . 0.940 no
C12 . H122 . 0.940 no
C13 . S1 . 1.636(2) yes
C13 . N2 . 1.165(3) yes
Cu1 . S1 5_465 3.0012(6) yes
Cu1 . N1 5_565 1.9882(10) yes
Cu1 . N1 . 1.9882(10) yes
Cu1 . N2 . 2.696(2) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 . O1 . C2 . 116.62(12) yes
C7 . O2 . Cu1 . 127.13(7) yes
O1 . C1 . H11 . 109.7 no
O1 . C1 . H12 . 109.7 no
H11 . C1 . H12 . 109.1 no
O1 . C1 . H13 . 106.5 no
H11 . C1 . H13 . 110.2 no
H12 . C1 . H13 . 111.5 no
O1 . C2 . C3 . 125.29(12) yes
O1 . C2 . C7 . 113.50(11) yes
C3 . C2 . C7 . 121.20(12) yes
C2 . C3 . C4 . 120.40(12) yes
C2 . C3 . H31 . 121.1 no
C4 . C3 . H31 . 118.5 no
C3 . C4 . C5 . 119.98(13) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 120.7 no
C4 . C5 . C6 . 120.56(13) yes
C4 . C5 . H51 . 120.7 no
C6 . C5 . H51 . 118.7 no
C5 . C6 . C7 . 120.52(11) yes
C5 . C6 . C8 . 117.09(11) yes
C7 . C6 . C8 . 121.57(10) yes
C2 . C7 . C6 . 117.24(11) yes
C2 . C7 . O2 . 118.07(10) yes
C6 . C7 . O2 . 124.65(10) yes
C6 . C8 . N1 . 127.91(10) yes
C6 . C8 . H81 . 114.2 no
N1 . C8 . H81 . 117.8 no
C10 . C9 . N1 . 115.77(11) yes
C10 . C9 . H91 . 110.7 no
N1 . C9 . H91 . 108.1 no
C10 . C9 . H92 . 104.7 no
N1 . C9 . H92 . 109.1 no
H91 . C9 . H92 . 108.1 no
C9 . C10 . C9 5_565 110.63(13) yes
C9 . C10 . C11 . 111.73(10) yes
C9 5_565 C10 . C11 . 111.73(10) yes
C9 . C10 . C12 . 106.54(10) yes
C9 5_565 C10 . C12 . 106.54(10) yes
C11 . C10 . C12 . 109.38(15) yes
C10 . C11 . H111 5_565 113.9 no
C10 . C11 . H111 . 113.9 no
H111 5_565 C11 . H111 . 104.2 no
C10 . C11 . H112 . 106.8 no
H111 5_565 C11 . H112 . 109.0 no
H111 . C11 . H112 . 109.0 no
C10 . C12 . H122 5_565 109.4 no
C10 . C12 . H121 . 110.0 no
H122 5_565 C12 . H121 . 109.3 no
C10 . C12 . H122 . 109.4 no
H122 5_565 C12 . H122 . 109.5 no
H121 . C12 . H122 . 109.3 no
S1 . C13 . N2 . 179.29(19) yes
S1 5_465 Cu1 . N1 5_565 86.47(3) yes
S1 5_465 Cu1 . O2 . 93.21(3) yes
N1 5_565 Cu1 . O2 . 173.49(4) yes
S1 5_465 Cu1 . O2 5_565 93.21(3) yes
N1 5_565 Cu1 . O2 5_565 92.01(4) yes
O2 . Cu1 . O2 5_565 81.51(5) yes
S1 5_465 Cu1 . N1 . 86.47(3) yes
N1 5_565 Cu1 . N1 . 94.47(6) yes
O2 . Cu1 . N1 . 92.01(4) yes
O2 5_565 Cu1 . N1 . 173.49(4) yes
S1 5_465 Cu1 . N2 . 177.63(4) yes
N1 5_565 Cu1 . N2 . 91.92(4) yes
O2 . Cu1 . N2 . 88.59(4) yes
O2 5_565 Cu1 . N2 . 88.59(4) yes
N1 . Cu1 . N2 . 91.92(4) yes
C13 . S1 . Cu1 1_655 115.66(7) yes
C9 . N1 . C8 . 115.70(10) yes
C9 . N1 . Cu1 . 122.01(8) yes
C8 . N1 . Cu1 . 122.26(8) yes
Cu1 . N2 . C13 . 118.75(16) yes
# Attachment '3910_web_deposit_cif_file_4_Jean-PascalSutter_1295611074.cif'
data_cpd1102
_database_code_depnum_ccdc_archive 'CCDC 809271'
#TrackingRef '3910_web_deposit_cif_file_4_Jean-PascalSutter_1295611074.cif'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107.
;
_refine_special_details
;
?
;
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 18.190(9)
_cell_length_b 18.190(9)
_cell_length_c 11.780(5)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 3376(3)
_symmetry_cell_setting trigonal
_symmetry_space_group_name_H-M 'P 31 2 1 '
_symmetry_space_group_name_Hall 'P 31 2" '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+y,-x,z+2/3
-x,-x+y,-z+1/3
-y,x-y,z+1/3
x-y,-y,-z+2/3
y,x,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841
1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 3
_chemical_formula_sum 'C40 H47 K1 N4 Ni2 O10'
_chemical_formula_moiety 'C40 H47 K1 N4 Ni2 O10'
_chemical_compound_source ?
_chemical_formula_weight 900.36
_cell_measurement_reflns_used 9625
_cell_measurement_theta_min 2
_cell_measurement_theta_max 28
_cell_measurement_temperature 110
_exptl_crystal_description stick
_exptl_crystal_colour red
_exptl_crystal_size_min 0.050
_exptl_crystal_size_mid 0.050
_exptl_crystal_size_max 0.300
_exptl_crystal_density_diffrn 1.329
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1401
_exptl_absorpt_coefficient_mu 0.985
# Sheldrick geometric approximatio 0.95 0.95
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min 0.86
_exptl_absorpt_correction_T_max 0.95
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 110
_diffrn_reflns_number 65962
_reflns_number_total 5715
_diffrn_reflns_av_R_equivalents 0.084
# Number of reflections without Friedels Law is 5715
# Number of reflections with Friedels Law is 3121
# Theoretical number of reflections is about 2875
_diffrn_reflns_theta_min 1.293
_diffrn_reflns_theta_max 28.583
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 28.011
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_reflns_limit_h_min -24
_reflns_limit_h_max 12
_reflns_limit_k_min 0
_reflns_limit_k_max 24
_reflns_limit_l_min 0
_reflns_limit_l_max 15
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.73
_refine_diff_density_max 1.06
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns 3624
_refine_ls_number_restraints 0
_refine_ls_number_parameters 262
_oxford_refine_ls_R_factor_ref 0.0797
_refine_ls_wR_factor_ref 0.0859
_refine_ls_goodness_of_fit_ref 1.0524
_refine_ls_shift/su_max 0.0002136
_refine_ls_shift/su_mean 0.0000109
# The values computed from all data
_oxford_reflns_number_all 5696
_refine_ls_R_factor_all 0.1189
_refine_ls_wR_factor_all 0.1274
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4037
_refine_ls_R_factor_gt 0.0862
_refine_ls_wR_factor_gt 0.0892
_refine_ls_abs_structure_Flack 0.01(3)
_refine_ls_abs_structure_details 'Flack (1983), 2576 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration ad
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
2.26 1.17 1.62
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.40991(6) 0.54078(6) 0.50771(6) 0.0416 1.0000 Uani . . . . . .
K1 K 0.64565(12) 0.64565(12) 0.5000 0.0434 1.0000 Uani S T . . . .
C1 C 0.4782(4) 0.6805(4) 0.3585(4) 0.0314 1.0000 Uani . . . . . .
C2 C 0.5455(5) 0.7601(4) 0.3236(4) 0.0376 1.0000 Uani . . . . . .
C3 C 0.5400(6) 0.8036(6) 0.2300(5) 0.0530 1.0000 Uani . . . . . .
C4 C 0.4607(7) 0.7651(7) 0.1687(5) 0.0639 1.0000 Uani . . . . . .
C5 C 0.3951(6) 0.6891(7) 0.1987(6) 0.0593 1.0000 Uani . . . . . .
C6 C 0.4018(5) 0.6445(6) 0.2944(5) 0.0487 1.0000 Uani . . . . . .
C7 C 0.3288(5) 0.5655(6) 0.3243(7) 0.0537 1.0000 Uani . . . . . .
C8 C 0.6872(6) 0.8687(6) 0.3559(7) 0.0619 1.0000 Uani . . . . . .
C9 C 0.2398(7) 0.4379(6) 0.4506(11) 0.0877 1.0000 Uani . . . . . .
C10 C 0.2646(8) 0.3843(8) 0.5055(13) 0.0960 1.0000 Uani . . . . . .
C11 C 0.1855(7) 0.3977(8) 0.3481(9) 0.0870 1.0000 Uani . . . . . .
C12 C 0.1967(5) 0.4672(6) 0.5437(8) 0.0601 1.0000 Uani . . . . . .
C13 C 0.4914(6) 0.5171(5) 0.6985(5) 0.0490 1.0000 Uani . . . . . .
C14 C 0.5605(6) 0.5471(6) 0.7719(5) 0.0527 1.0000 Uani . . . . . .
C15 C 0.5607(8) 0.4996(7) 0.8642(6) 0.0798 1.0000 Uani . . . . . .
C16 C 0.4937(11) 0.4222(9) 0.8878(10) 0.0958 1.0000 Uani . . . . . .
C17 C 0.4249(10) 0.3907(7) 0.8194(11) 0.0935 1.0000 Uani . . . . . .
C18 C 0.4194(6) 0.4368(5) 0.7223(7) 0.0600 1.0000 Uani . . . . . .
C19 C 0.3458(7) 0.4026(5) 0.6551(8) 0.0753 1.0000 Uani . . . . . .
C20 C 0.6951(6) 0.6640(7) 0.8218(5) 0.0631 1.0000 Uani . . . . . .
N1 N 0.3243(4) 0.5185(4) 0.4071(7) 0.0575 1.0000 Uani . . . . . .
N2 N 0.3344(5) 0.4376(5) 0.5675(6) 0.0714 1.0000 Uani . . . . . .
O1 O 0.4875(3) 0.6445(3) 0.4470(3) 0.0367 1.0000 Uani . . . . . .
O2 O 0.4934(3) 0.5641(3) 0.6124(3) 0.0424 1.0000 Uani . . . . . .
O3 O 0.6164(3) 0.7890(3) 0.3893(4) 0.0462 1.0000 Uani . . . . . .
O4 O 0.6263(4) 0.6236(4) 0.7429(3) 0.0485 1.0000 Uani . . . . . .
O5 O 0.7825(11) 0.8129(13) 0.5811(18) 0.1126 0.5000 Uani . . . . . .
O6 O 0.9894(15) 0.8003(11) 0.9248(18) 0.1230 0.5000 Uani . . . . . .
H31 H 0.5855 0.8563 0.2088 0.0607 1.0000 Uiso R . . . . .
H41 H 0.4547 0.7934 0.1064 0.0728 1.0000 Uiso R . . . . .
H51 H 0.3450 0.6661 0.1580 0.0742 1.0000 Uiso R . . . . .
H71 H 0.2795 0.5459 0.2802 0.0623 1.0000 Uiso R . . . . .
H81 H 0.7319 0.8881 0.4110 0.0948 1.0000 Uiso R . . . . .
H82 H 0.6707 0.9111 0.3482 0.0946 1.0000 Uiso R . . . . .
H83 H 0.7101 0.8640 0.2839 0.0947 1.0000 Uiso R . . . . .
H112 H 0.1683 0.4354 0.3145 0.1331 1.0000 Uiso R . . . . .
H111 H 0.1362 0.3462 0.3746 0.1329 1.0000 Uiso R . . . . .
H113 H 0.2163 0.3839 0.2925 0.1330 1.0000 Uiso R . . . . .
H123 H 0.1618 0.4862 0.5077 0.0880 1.0000 Uiso R . . . . .
H121 H 0.2397 0.5126 0.5876 0.0879 1.0000 Uiso R . . . . .
H122 H 0.1614 0.4193 0.5915 0.0885 1.0000 Uiso R . . . . .
H151 H 0.6086 0.5217 0.9107 0.0932 1.0000 Uiso R . . . . .
H161 H 0.4946 0.3915 0.9508 0.1120 1.0000 Uiso R . . . . .
H171 H 0.3791 0.3366 0.8355 0.1120 1.0000 Uiso R . . . . .
H191 H 0.3009 0.3499 0.6764 0.0870 1.0000 Uiso R . . . . .
H202 H 0.7377 0.7184 0.7928 0.0980 1.0000 Uiso R . . . . .
H201 H 0.6743 0.6713 0.8945 0.0978 1.0000 Uiso R . . . . .
H203 H 0.7202 0.6290 0.8320 0.0979 1.0000 Uiso R . . . . .
H101 H 0.2206 0.3490 0.5540 0.1299 1.0000 Uiso R . . . . .
H102 H 0.2728 0.3547 0.4540 0.1299 1.0000 Uiso . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0448(5) 0.0476(5) 0.0301(3) -0.0032(4) 0.0081(3) 0.0213(4)
K1 0.0563(9) 0.0563(9) 0.0190(6) 0.0010(4) -0.0010(4) 0.0293(11)
C1 0.049(4) 0.040(3) 0.019(2) -0.008(2) -0.001(2) 0.031(3)
C2 0.064(4) 0.050(4) 0.017(2) -0.004(2) 0.000(2) 0.042(4)
C3 0.089(6) 0.077(5) 0.023(2) 0.012(3) 0.015(3) 0.064(5)
C4 0.109(8) 0.106(7) 0.020(3) -0.001(4) -0.007(4) 0.087(7)
C5 0.080(6) 0.106(7) 0.021(3) -0.013(4) -0.013(3) 0.069(6)
C6 0.063(5) 0.084(6) 0.027(3) -0.020(3) -0.017(3) 0.058(5)
C7 0.050(4) 0.067(5) 0.058(5) -0.031(4) -0.022(3) 0.040(4)
C8 0.069(5) 0.054(5) 0.049(4) 0.009(4) 0.018(4) 0.019(4)
C9 0.055(4) 0.058(4) 0.135(7) -0.023(4) -0.014(4) 0.017(3)
C10 0.063(4) 0.066(4) 0.144(7) -0.023(4) -0.014(4) 0.021(3)
C11 0.075(7) 0.095(8) 0.072(6) -0.017(6) -0.003(5) 0.028(6)
C12 0.043(4) 0.076(6) 0.064(5) -0.008(4) 0.007(4) 0.032(4)
C13 0.087(6) 0.057(4) 0.024(3) 0.006(3) 0.017(3) 0.051(4)
C14 0.089(6) 0.086(6) 0.019(3) 0.013(3) 0.016(3) 0.070(5)
C15 0.142(10) 0.119(9) 0.032(3) 0.037(4) 0.042(5) 0.105(8)
C16 0.175(14) 0.122(11) 0.059(6) 0.053(7) 0.062(8) 0.126(12)
C17 0.168(13) 0.066(6) 0.081(7) 0.042(6) 0.081(9) 0.084(8)
C18 0.087(6) 0.041(4) 0.045(4) 0.009(3) 0.043(4) 0.026(4)
C19 0.088(7) 0.038(4) 0.057(5) -0.008(4) 0.039(5) 0.000(5)
C20 0.083(6) 0.109(8) 0.027(3) -0.012(4) -0.014(3) 0.070(6)
N1 0.046(4) 0.046(4) 0.079(5) -0.021(3) -0.010(3) 0.021(3)
N2 0.070(5) 0.061(4) 0.042(3) -0.004(3) 0.030(3) 0.002(4)
O1 0.042(2) 0.044(3) 0.0278(19) 0.0057(18) 0.0008(17) 0.024(2)
O2 0.060(3) 0.044(3) 0.0188(16) 0.0089(17) 0.0072(17) 0.022(2)
O3 0.056(3) 0.048(3) 0.028(2) 0.0069(19) 0.009(2) 0.022(2)
O4 0.072(3) 0.077(3) 0.0189(17) 0.0013(19) 0.0001(19) 0.053(3)
O5 0.071(10) 0.122(14) 0.125(14) 0.026(12) -0.008(10) 0.034(10)
O6 0.147(18) 0.074(10) 0.119(15) 0.028(10) 0.040(13) 0.033(11)
_refine_ls_extinction_method None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . N1 . 1.833(7) yes
Ni1 . N2 . 1.823(7) yes
Ni1 . O1 . 1.844(5) yes
Ni1 . O2 . 1.834(5) yes
C1 . C2 . 1.410(10) yes
C1 . C6 . 1.422(10) yes
C1 . O1 . 1.286(7) yes
C2 . C3 . 1.391(8) yes
C2 . O3 . 1.364(8) yes
C3 . C4 . 1.443(13) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.346(14) yes
C4 . H41 . 0.934 no
C5 . C6 . 1.428(11) yes
C5 . H51 . 0.924 no
C6 . C7 . 1.430(13) yes
C7 . N1 . 1.273(12) yes
C7 . H71 . 0.939 no
C8 . O3 . 1.431(9) yes
C8 . H81 . 0.959 no
C8 . H82 . 0.962 no
C8 . H83 . 0.968 no
C9 . C10 . 1.418(18) yes
C9 . C11 . 1.498(15) yes
C9 . C12 . 1.588(14) yes
C9 . N1 . 1.588(13) yes
C10 . N2 . 1.362(14) yes
C10 . H101 . 0.930 no
C10 . H102 . 0.872 no
C11 . H112 . 0.970 no
C11 . H111 . 0.970 no
C11 . H113 . 0.973 no
C12 . H123 . 0.959 no
C12 . H121 . 0.957 no
C12 . H122 . 0.963 no
C13 . C14 . 1.393(12) yes
C13 . C18 . 1.420(12) yes
C13 . O2 . 1.315(8) yes
C14 . C15 . 1.389(10) yes
C14 . O4 . 1.350(11) yes
C15 . C16 . 1.352(18) yes
C15 . H151 . 0.933 no
C16 . C17 . 1.35(2) yes
C16 . H161 . 0.934 no
C17 . C18 . 1.450(15) yes
C17 . H171 . 0.938 no
C18 . C19 . 1.404(15) yes
C19 . N2 . 1.283(14) yes
C19 . H191 . 0.931 no
C20 . O4 . 1.432(9) yes
C20 . H202 . 0.964 no
C20 . H201 . 0.972 no
C20 . H203 . 0.959 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ni1 . N2 . 84.4(4) yes
N1 . Ni1 . O1 . 96.1(3) yes
N2 . Ni1 . O1 . 179.0(3) yes
N1 . Ni1 . O2 . 177.8(3) yes
N2 . Ni1 . O2 . 95.1(3) yes
O1 . Ni1 . O2 . 84.38(19) yes
C2 . C1 . C6 . 117.7(6) yes
C2 . C1 . O1 . 119.4(6) yes
C6 . C1 . O1 . 122.9(6) yes
C1 . C2 . C3 . 122.9(7) yes
C1 . C2 . O3 . 113.5(5) yes
C3 . C2 . O3 . 123.6(7) yes
C2 . C3 . C4 . 117.4(8) yes
C2 . C3 . H31 . 121.2 no
C4 . C3 . H31 . 121.5 no
C3 . C4 . C5 . 121.6(7) yes
C3 . C4 . H41 . 119.3 no
C5 . C4 . H41 . 119.0 no
C4 . C5 . C6 . 120.5(8) yes
C4 . C5 . H51 . 119.7 no
C6 . C5 . H51 . 119.8 no
C5 . C6 . C1 . 119.9(8) yes
C5 . C6 . C7 . 117.7(8) yes
C1 . C6 . C7 . 122.3(7) yes
C6 . C7 . N1 . 125.4(7) yes
C6 . C7 . H71 . 118.4 no
N1 . C7 . H71 . 116.2 no
O3 . C8 . H81 . 110.8 no
O3 . C8 . H82 . 110.9 no
H81 . C8 . H82 . 108.4 no
O3 . C8 . H83 . 111.2 no
H81 . C8 . H83 . 107.5 no
H82 . C8 . H83 . 108.0 no
C10 . C9 . C11 . 113.0(10) yes
C10 . C9 . C12 . 107.2(11) yes
C11 . C9 . C12 . 113.8(9) yes
C10 . C9 . N1 . 106.8(9) yes
C11 . C9 . N1 . 106.7(10) yes
C12 . C9 . N1 . 109.0(7) yes
C9 . C10 . N2 . 104.9(10) yes
C9 . C10 . H101 . 107.1 no
N2 . C10 . H101 . 109.7 no
C9 . C10 . H102 . 108.5 no
N2 . C10 . H102 . 115.2 no
H101 . C10 . H102 . 110.9 no
C9 . C11 . H112 . 110.6 no
C9 . C11 . H111 . 106.1 no
H112 . C11 . H111 . 110.2 no
C9 . C11 . H113 . 110.2 no
H112 . C11 . H113 . 109.8 no
H111 . C11 . H113 . 109.8 no
C9 . C12 . H123 . 110.1 no
C9 . C12 . H121 . 109.5 no
H123 . C12 . H121 . 109.3 no
C9 . C12 . H122 . 108.5 no
H123 . C12 . H122 . 108.8 no
H121 . C12 . H122 . 110.6 no
C14 . C13 . C18 . 117.9(7) yes
C14 . C13 . O2 . 119.9(7) yes
C18 . C13 . O2 . 122.2(8) yes
C13 . C14 . C15 . 121.6(9) yes
C13 . C14 . O4 . 114.1(6) yes
C15 . C14 . O4 . 124.3(9) yes
C14 . C15 . C16 . 121.8(12) yes
C14 . C15 . H151 . 118.9 no
C16 . C15 . H151 . 119.3 no
C15 . C16 . C17 . 118.7(9) yes
C15 . C16 . H161 . 120.6 no
C17 . C16 . H161 . 120.7 no
C16 . C17 . C18 . 122.8(11) yes
C16 . C17 . H171 . 118.1 no
C18 . C17 . H171 . 119.0 no
C17 . C18 . C13 . 117.1(10) yes
C17 . C18 . C19 . 121.0(10) yes
C13 . C18 . C19 . 121.9(8) yes
C18 . C19 . N2 . 126.1(7) yes
C18 . C19 . H191 . 117.1 no
N2 . C19 . H191 . 116.8 no
O4 . C20 . H202 . 110.0 no
O4 . C20 . H201 . 109.9 no
H202 . C20 . H201 . 109.8 no
O4 . C20 . H203 . 109.0 no
H202 . C20 . H203 . 108.8 no
H201 . C20 . H203 . 109.3 no
C9 . N1 . C7 . 125.1(8) yes
C9 . N1 . Ni1 . 108.6(7) yes
C7 . N1 . Ni1 . 125.8(6) yes
C10 . N2 . C19 . 113.7(9) yes
C10 . N2 . Ni1 . 118.7(8) yes
C19 . N2 . Ni1 . 126.6(7) yes
C1 . O1 . Ni1 . 127.4(4) yes
C13 . O2 . Ni1 . 128.1(5) yes
C8 . O3 . C2 . 115.6(6) yes
C20 . O4 . C14 . 117.5(6) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C19 . H191 . O6 5_566 174 0.93 2.58 3.504(15) yes