# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Euan Brechin'
_publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK
_publ_section_title
;
High pressure effects on a trimetallic MnII/III SMM
;
_publ_requested_coeditor_name A.Prescimone@sms.ed.ac.uk
loop_
_publ_author_name
'Euan Brechin'
'Konstantin V. Kamenev'
'Mark Murrie'
'Simon Parsons'
'Alessandro Prescimone'
;
J.Sanchez-Benitez
;
# Attachment 'mcht01.cif'
data_mcht01
_database_code_depnum_ccdc_archive 'CCDC 730663'
#0.16 GPa data set.
_audit_creation_date 08-12-17
_audit_creation_method CRYSTALS_ver_12.86
_oxford_structure_analysis_title 'mcht01b in I2/m'
_chemical_name_systematic ?
_chemical_melting_point ?
_chemical_compound_source 'Alessandro Prescimone'
_publ_section_exptl_refinement
;
H atoms placed geometrically after each cycle on carbon.
Those attached to O were located from H-bonding considerations
and allowed to ride on their parent O-atoms.
Checkcif output:
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.69
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 11.82 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.73
088_ALERT_3_A Poor Data / Parameter Ratio .................... 5.18
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.555 796
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 1
These alerts all derive from shading of reciprocal space by the pressure cell,
and they are unavoidable in high pressure crystal structure determinations.
023_ALERT_3_B Resolution (too) Low [sin(th)/Lambda < 0.6]..... 15.35 Deg.
Rint and Rsigma increase sharply beyond 0.9 Ang. resolution.
INTENSITY STATISTICS FOR DATASET # 1 mcht01.hkl
Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma
Inf - 2.25 125 180 69.4 4.52 122.5 40.82 0.0284 0.0217
2.25 - 1.78 128 171 74.9 4.04 84.4 30.19 0.0327 0.0245
1.78 - 1.55 133 177 75.1 3.90 57.3 23.49 0.0442 0.0337
1.55 - 1.40 134 189 70.9 3.60 37.8 19.30 0.0562 0.0414
1.40 - 1.30 130 176 73.9 3.40 28.2 14.72 0.0797 0.0572
1.30 - 1.22 135 187 72.2 3.42 17.3 10.19 0.1041 0.0841
1.22 - 1.16 128 178 71.9 3.40 11.2 7.55 0.1415 0.1251
1.16 - 1.10 136 204 66.7 3.02 8.5 5.57 0.1898 0.1755
1.10 - 1.06 124 182 68.1 3.07 7.0 4.44 0.2401 0.2199
1.06 - 1.02 136 195 69.7 2.92 7.6 4.47 0.2324 0.2207
1.02 - 0.98 156 233 67.0 2.76 6.5 3.39 0.3741 0.2778
0.98 - 0.95 127 204 62.3 2.55 4.9 2.86 0.3386 0.3552
0.95 - 0.92 149 231 64.5 2.42 3.8 2.17 0.3912 0.4908
0.92 - 0.89 159 256 62.1 2.45 2.5 1.37 0.6062 0.7466
0.89 - 0.86 174 301 57.8 2.04 2.2 1.12 0.6808 0.9246
0.86 - 0.84 137 224 61.2 2.30 2.0 1.00 0.7250 1.0484
0.84 - 0.82 141 253 55.7 1.98 1.7 0.86 0.7776 1.2289
0.82 - 0.80 90 180 50.0 1.30 1.5 0.59 0.7836 1.8423
0.90 - 0.80 655 1135 57.7 2.05 2.0 1.02 0.6911 1.0489
Inf - 0.80 2442 3721 65.6 2.87 21.7 9.33 0.0761 0.0857
601_ALERT_2_A Structure Contains Solvent Accessible VOIDS of . 325.00 A**3
In the ambient structure there is presence of 2 half occupied CH3CN
molecules per complex molecule. At high pressure no extra peaks assignable to
solvent are present in the difference map. Forcing the presence of a solvent
molecule in the same position as in the ambient structure doesn't improve the
R-factor and actually refines to an occupancy very close to zero. We should
therefore assume that the solvent has been squeezed out of the crystal as
effect of the high pressure.
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
the reported formula takes in account the solvent molecule that is actually not
present in the crystal anymore.
910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 1
913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 44
Very strong reflections overload the detector pixels with synchrotron
radiation.
420_ALERT_2_B D-H Without Acceptor O20 - H201 ... ?
No suitable acceptors were found at reasonable orientation, the H-atom has been
positioned geometrically.
432_ALERT_2_B Short Inter X...Y Contact O23 .. C4 .. 2.90 Ang.
This is a contact between a disordered Oxygen from a perchlorate and an
aromatic CH group. These contacts can not be avoided.
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . CL26
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O27
the occupancy for these atoms is set to be less than 1 despite being on a
special position because in the overall formula there must be 3 perchlorates
to keep the charges balanced. With the occupancy set to 0.5 the R-factor is
lower than the full occupancy case.
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O28
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O29
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O30
These alert is due the program getting confused from the disordered Oxygens
atom on a perchlorate anion: in fact these atoms do not have three covalents
bonds but only one with a Chlorine atom.
128_ALERT_4_C Non-standard setting of Space group C2/m .... I2/m
This setting has been chosen to keep the model of the structure consistent with
ambient pressure structure already present in literature.
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C6
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7
Some atoms on an aromati ring show high thermal motion, this is not
unexpected or unusal for this type of structure.
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl21
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl26
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1
these are quite heavy atoms with an higher coordiantion number compared to
the atoms are attached to: therefore this effect is not surprising.
302_ALERT_4_C Anion/Solvent Disorder ......................... 34.00 Perc.
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C4
341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 16
No action taken here.
;
#end of refcif
_cell_length_a 11.897(2)
_cell_length_b 22.067(4)
_cell_length_c 13.312(3)
_cell_angle_alpha 90
_cell_angle_beta 93.82(3)
_cell_angle_gamma 90
_cell_volume 3487.0(12)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'I 1 2/m 1 '
_symmetry_space_group_name_Hall '-I 2y'
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,-z
x,-y,z
-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 0.0000 0.0010 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'
N 0.0010 0.0010 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 0.0030 0.0030 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'
Cl 0.0750 0.0710 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.2220 0.3450 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C54 H54 Cl3 Mn3 N9 O18
# Dc = 1.32 Fooo = 1380.00 Mu = 7.18 M = 347.05
# Found Formula = C52 H52 Cl3 Mn3 N8 O18
# Dc = 1.28 FOOO = 1380.00 Mu = 7.15 M = 337.04
_chemical_formula_sum 'C52 H52 Cl3 Mn3 N8 O18'
_chemical_formula_moiety '[Mn3(BPy)4(cht)2][ClO4]3'
_chemical_formula_weight 1348.17
_cell_measurement_reflns_used 1658
_cell_measurement_theta_min 2
_cell_measurement_theta_max 17
_cell_measurement_temperature 300
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_min 0.08
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_max 0.11
_exptl_crystal_density_diffrn 1.284
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1380
_exptl_absorpt_coefficient_mu 0.715
# Sheldrick geometric approximatio 0.93 0.94
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.45
_exptl_absorpt_correction_T_max 0.94
_diffrn_measurement_device 'Bruker SMART APEX-II on Station 9.8, SRS'
_diffrn_measurement_device_type Area
_diffrn_radiation_monochromator silicon
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.47670
_diffrn_measurement_method \w
# 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 ?
_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 300
_diffrn_ambient_pressure 160000
_diffrn_reflns_number 8357
_reflns_number_total 1787
_diffrn_reflns_av_R_equivalents 0.071
# Number of reflections with Friedels Law is 1787
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 2482
_diffrn_reflns_theta_min 1.238
_diffrn_reflns_theta_max 15.352
_diffrn_measured_fraction_theta_max 0.692
_diffrn_reflns_theta_full 11.821
_diffrn_measured_fraction_theta_full 0.725
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -13
_reflns_limit_h_max 13
_reflns_limit_k_min -24
_reflns_limit_k_max 24
_reflns_limit_l_min -11
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary 'From ambient pressure structure'
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.30
_refine_diff_density_max 0.33
# 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>2.0\s(I)
_refine_ls_number_reflns 1011
_refine_ls_number_restraints 32
_refine_ls_number_parameters 195
_oxford_refine_ls_R_factor_ref 0.0735
_refine_ls_wR_factor_ref 0.0417
_refine_ls_goodness_of_fit_ref 0.9750
_refine_ls_shift/su_max 0.006214
# The values computed from all data
_oxford_reflns_number_all 1613
_refine_ls_R_factor_all 0.1242
_refine_ls_wR_factor_all 0.0464
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 1011
_refine_ls_R_factor_gt 0.0735
_refine_ls_wR_factor_gt 0.0417
# 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 sigma
_refine_ls_weighting_details
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;
# 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.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
;
# 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
Mn1 Mn 1.0000 0.5000 0.5000 0.0554 1.0000 Uani S T . . . . .
Mn2 Mn 1.0000 0.64141(6) 0.5000 0.0600 1.0000 Uani S T . . . . .
O15 O 1.0979(3) 0.56328(16) 0.4668(4) 0.0638 1.0000 Uani . . . . . . .
C16 C 1.1776(6) 0.5568(2) 0.3926(10) 0.0683 1.0000 Uani . . . . . . .
C17 C 1.2472(7) 0.500000(6) 0.4127(11) 0.0793 1.0000 Uani S T . . . . .
C18 C 1.1179(7) 0.5561(3) 0.2875(9) 0.0754 1.0000 Uani . . . . . . .
C19 C 1.0573(9) 0.500000(7) 0.2716(13) 0.0831 1.0000 Uani S T . . . . .
O20 O 0.9515(6) 0.500000(7) 0.3277(7) 0.0841 1.0000 Uani S T . . . . .
Cl21 Cl 0.0000 0.14421(12) 0.0000 0.0795 1.0000 Uani DS T . . . . .
O22 O 0.0000 0.2070(3) 0.0000 0.207(3) 1.0000 Uiso DS . . . . . .
O23 O -0.0819(18) 0.1259(6) 0.0626(19) 0.207(3) 0.5000 Uiso D . . . . . .
O24 O -0.027(2) 0.1231(6) -0.0952(8) 0.207(3) 0.5000 Uiso D . . . . . .
O25 O 0.1023(10) 0.1234(5) 0.036(2) 0.207(3) 0.5000 Uiso D . . . . . .
Cl26 Cl 0.5000 0.3960(5) 0.0000 0.231(5) 0.5000 Uiso DS . . . . . .
O27 O 0.5000 0.3324(6) 0.0000 0.279(11) 0.5000 Uiso DS . . . . . .
O28 O 0.545(8) 0.4179(8) -0.088(3) 0.279(11) 0.2500 Uiso D . . . 1 . .
O29 O 0.562(7) 0.4178(9) 0.086(4) 0.279(11) 0.2500 Uiso D . . . 1 . .
O30 O 0.3873(12) 0.4166(9) 0.002(8) 0.279(11) 0.2500 Uiso D . . . 1 . .
N3 N 1.1109(5) 0.6615(2) 0.6381(6) 0.0724 1.0000 Uani . . . . . . .
C4 C 1.2087(6) 0.6304(3) 0.6614(10) 0.0893 1.0000 Uani . . . . . . .
C5 C 1.2708(8) 0.6419(5) 0.7479(13) 0.1109 1.0000 Uani . . . . . . .
C6 C 1.2325(11) 0.6773(6) 0.8182(13) 0.1339 1.0000 Uani . . . . . . .
C7 C 1.1298(10) 0.7091(4) 0.7886(13) 0.1198 1.0000 Uani . . . . . . .
C8 C 1.0706(7) 0.7001(4) 0.7060(10) 0.0646 1.0000 Uani . . . . . . .
C9 C 0.9674(7) 0.7316(3) 0.6743(10) 0.0829 1.0000 Uani . . . . . . .
C10 C 0.9343(8) 0.7822(3) 0.7312(9) 0.0993 1.0000 Uani . . . . . . .
C11 C 0.8320(9) 0.8081(4) 0.6975(12) 0.1183 1.0000 Uani . . . . . . .
C12 C 0.7714(8) 0.7852(5) 0.6120(12) 0.1189 1.0000 Uani D . . . . . .
C13 C 0.8098(7) 0.7355(3) 0.5663(8) 0.1028 1.0000 Uani D . . . . . .
N14 N 0.9074(6) 0.7099(3) 0.5933(7) 0.0724 1.0000 Uani . . . . . . .
H161 H 1.2263 0.5909 0.3968 0.0500 1.0000 Uiso R . . . . . .
H171 H 1.2765 0.5000 0.4808 0.0500 1.0000 Uiso RS . . . . . .
H172 H 1.3077 0.5000 0.3695 0.0500 1.0000 Uiso RS . . . . . .
H181 H 1.1729 0.5592 0.2393 0.0500 1.0000 Uiso R . . . . . .
H182 H 1.0674 0.5894 0.2800 0.0500 1.0000 Uiso R . . . . . .
H191 H 1.0304 0.5000 0.2028 0.0500 1.0000 Uiso RS . . . . . .
H41 H 1.2341 0.6014 0.6152 0.0500 1.0000 Uiso R . . . . . .
H51 H 1.3423 0.6231 0.7599 0.0500 1.0000 Uiso R . . . . . .
H61 H 1.2707 0.6819 0.8827 0.0500 1.0000 Uiso R . . . . . .
H71 H 1.1023 0.7374 0.8349 0.0500 1.0000 Uiso R . . . . . .
H101 H 0.9778 0.7978 0.7878 0.0500 1.0000 Uiso R . . . . . .
H111 H 0.8018 0.8405 0.7342 0.0500 1.0000 Uiso R . . . . . .
H121 H 0.7050 0.8051 0.5857 0.0500 1.0000 Uiso R . . . . . .
H131 H 0.7637 0.7175 0.5134 0.0500 1.0000 Uiso R . . . . . .
H201 H 0.8804 0.5000 0.3001 0.0500 1.0000 Uiso RS . . . . . .
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
Mn1 0.0567(11) 0.0417(12) 0.069(3) 0.0000 0.0157(13) 0.0000
Mn2 0.0741(9) 0.0408(8) 0.065(2) 0.0000 0.0035(9) 0.0000
O15 0.071(3) 0.038(3) 0.083(6) 0.008(2) 0.013(3) -0.0096(18)
C16 0.063(4) 0.044(4) 0.101(13) 0.002(4) 0.024(5) -0.003(3)
C17 0.067(5) 0.065(6) 0.110(17) 0.0000 0.032(7) 0.0000
C18 0.111(6) 0.067(6) 0.052(13) 0.009(4) 0.032(6) 0.010(4)
C19 0.111(8) 0.066(7) 0.075(18) 0.0000 0.027(9) 0.0000
O20 0.094(4) 0.075(5) 0.082(12) 0.0000 0.001(5) 0.0000
Cl21 0.0730(13) 0.0876(19) 0.079(5) 0.0000 0.0134(17) 0.0000
N3 0.092(4) 0.057(4) 0.066(10) -0.003(3) -0.008(4) -0.016(3)
C4 0.076(5) 0.087(6) 0.104(15) -0.015(5) -0.007(6) 0.002(5)
C5 0.101(6) 0.123(9) 0.103(18) -0.001(8) -0.034(8) 0.013(6)
C6 0.155(11) 0.137(10) 0.10(2) -0.016(10) -0.040(10) 0.001(8)
C7 0.153(9) 0.084(7) 0.12(2) -0.029(7) 0.018(9) -0.002(7)
C8 0.083(5) 0.074(6) 0.035(12) -0.019(5) -0.011(5) -0.013(4)
C9 0.103(6) 0.056(5) 0.095(14) -0.010(5) 0.041(6) -0.016(5)
C10 0.133(7) 0.092(7) 0.074(15) -0.036(6) 0.008(7) 0.020(5)
C11 0.157(9) 0.077(6) 0.127(18) -0.021(6) 0.056(8) 0.028(7)
C12 0.107(7) 0.126(9) 0.127(19) -0.014(8) 0.030(8) 0.047(6)
C13 0.075(5) 0.075(6) 0.159(15) 0.009(6) 0.016(6) -0.003(4)
N14 0.092(5) 0.068(4) 0.056(10) -0.003(3) -0.003(5) 0.007(4)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.4850(18)
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
Mn1 . O20 2_766 2.327(9) yes
Mn1 . O15 6_565 1.889(4) yes
Mn1 . O15 2_766 1.889(4) yes
Mn1 . O15 5_756 1.889(4) yes
Mn1 . O15 . 1.889(4) yes
Mn1 . O20 . 2.327(9) yes
Mn2 . N3 5_756 2.235(7) yes
Mn2 . O15 5_756 2.143(4) yes
Mn2 . N14 5_756 2.286(7) yes
Mn2 . O15 . 2.143(4) yes
Mn2 . N3 . 2.235(7) yes
Mn2 . N14 . 2.286(7) yes
O15 . C16 . 1.422(10) yes
C16 . C17 . 1.516(7) yes
C16 . C18 . 1.525(12) yes
C16 . H161 . 0.950 no
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.441(8) yes
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C19 . O20 . 1.505(13) yes
C19 . H191 . 0.950 no
O20 . H201 . 0.900 no
Cl21 . O23 5_555 1.384(6) yes
Cl21 . O24 5_555 1.369(7) yes
Cl21 . O25 5_555 1.359(7) yes
Cl21 . O22 . 1.385(6) yes
Cl21 . O23 . 1.384(6) yes
Cl21 . O24 . 1.369(7) yes
Cl21 . O25 . 1.359(7) yes
O23 . O24 5_555 1.344(14) yes
O23 . O25 5_555 1.322(19) yes
O24 . O25 5_555 1.228(17) yes
Cl26 . O30 5_655 1.417(8) yes
Cl26 . O28 5_655 1.403(6) yes
Cl26 . O29 5_655 1.402(6) yes
Cl26 . O27 . 1.404(8) yes
Cl26 . O28 . 1.403(6) yes
Cl26 . O29 . 1.402(6) yes
Cl26 . O30 . 1.417(8) yes
O28 . O30 5_655 1.35(2) yes
O28 . O29 5_655 1.28(2) yes
O29 . O30 5_655 1.34(2) yes
N3 . C4 . 1.369(8) yes
N3 . C8 . 1.352(11) yes
C4 . C5 . 1.350(16) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.323(17) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.442(13) yes
C6 . H61 . 0.950 no
C7 . C8 . 1.282(14) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.450(11) yes
C9 . C10 . 1.419(11) yes
C9 . N14 . 1.341(11) yes
C10 . C11 . 1.392(11) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.401(15) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.348(8) yes
C12 . H121 . 0.950 no
C13 . N14 . 1.319(8) yes
C13 . H131 . 0.950 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
O20 2_766 Mn1 . O15 6_565 96.6(2) yes
O20 2_766 Mn1 . O15 2_766 83.4(2) yes
O15 6_565 Mn1 . O15 2_766 84.7(3) yes
O20 2_766 Mn1 . O15 5_756 83.4(2) yes
O15 6_565 Mn1 . O15 5_756 179.994 yes
O15 2_766 Mn1 . O15 5_756 95.3(3) yes
O20 2_766 Mn1 . O15 . 96.6(2) yes
O15 6_565 Mn1 . O15 . 95.3(3) yes
O15 2_766 Mn1 . O15 . 179.994 yes
O15 5_756 Mn1 . O15 . 84.7(3) yes
O20 2_766 Mn1 . O20 . 179.995 yes
O15 6_565 Mn1 . O20 . 83.4(2) yes
O15 2_766 Mn1 . O20 . 96.6(2) yes
O15 5_756 Mn1 . O20 . 96.6(2) yes
O15 . Mn1 . O20 . 83.4(2) yes
N3 5_756 Mn2 . O15 5_756 91.7(2) yes
N3 5_756 Mn2 . N14 5_756 72.6(3) yes
O15 5_756 Mn2 . N14 5_756 158.8(3) yes
N3 5_756 Mn2 . O15 . 106.8(2) yes
O15 5_756 Mn2 . O15 . 72.8(2) yes
N14 5_756 Mn2 . O15 . 97.6(2) yes
N3 5_756 Mn2 . N3 . 157.1(3) yes
O15 5_756 Mn2 . N3 . 106.8(2) yes
N14 5_756 Mn2 . N3 . 92.1(3) yes
O15 . Mn2 . N3 . 91.7(2) yes
N3 5_756 Mn2 . N14 . 92.1(3) yes
O15 5_756 Mn2 . N14 . 97.6(2) yes
N14 5_756 Mn2 . N14 . 97.2(4) yes
O15 . Mn2 . N14 . 158.8(3) yes
N3 . Mn2 . N14 . 72.6(3) yes
Mn2 . O15 . Mn1 . 101.2(2) yes
Mn2 . O15 . C16 . 128.4(3) yes
Mn1 . O15 . C16 . 122.5(4) yes
O15 . C16 . C17 . 110.1(8) yes
O15 . C16 . C18 . 110.3(6) yes
C17 . C16 . C18 . 111.7(8) yes
O15 . C16 . H161 . 108.1 no
C17 . C16 . H161 . 108.7 no
C18 . C16 . H161 . 107.9 no
C16 . C17 . C16 6_565 111.5(7) yes
C16 . C17 . H171 . 109.3 no
C16 6_565 C17 . H171 . 109.3 no
C16 . C17 . H172 . 108.7 no
C16 6_565 C17 . H172 . 108.7 no
H171 . C17 . H172 . 109.5 no
C16 . C18 . C19 . 109.9(8) yes
C16 . C18 . H181 . 108.6 no
C19 . C18 . H181 . 108.8 no
C16 . C18 . H182 . 110.0 no
C19 . C18 . H182 . 110.0 no
H181 . C18 . H182 . 109.5 no
C18 . C19 . C18 6_565 118.4(9) yes
C18 . C19 . O20 . 110.7(7) yes
C18 6_565 C19 . O20 . 110.7(7) yes
C18 . C19 . H191 . 106.0 no
C18 6_565 C19 . H191 . 106.0 no
O20 . C19 . H191 . 103.8 no
C19 . O20 . Mn1 . 109.2(7) yes
C19 . O20 . H201 . 126.2 no
Mn1 . O20 . H201 . 124.6 no
O23 5_555 Cl21 . O24 5_555 109.0(6) yes
O23 5_555 Cl21 . O25 5_555 109.8(7) yes
O24 5_555 Cl21 . O25 5_555 111.4(6) yes
O23 5_555 Cl21 . O22 . 106.9(5) yes
O24 5_555 Cl21 . O22 . 109.9(6) yes
O25 5_555 Cl21 . O22 . 109.8(5) yes
O23 5_555 Cl21 . O23 . 146.1(11) yes
O24 5_555 Cl21 . O23 . 58.4(6) yes
O25 5_555 Cl21 . O23 . 57.6(8) yes
O22 . Cl21 . O23 . 106.9(5) yes
O23 5_555 Cl21 . O24 . 58.4(6) yes
O24 5_555 Cl21 . O24 . 140.2(12) yes
O25 5_555 Cl21 . O24 . 53.5(7) yes
O22 . Cl21 . O24 . 109.9(6) yes
O23 . Cl21 . O24 . 109.0(6) yes
O23 5_555 Cl21 . O25 . 57.6(8) yes
O24 5_555 Cl21 . O25 . 53.5(7) yes
O25 5_555 Cl21 . O25 . 140.4(11) yes
O22 . Cl21 . O25 . 109.8(5) yes
O23 . Cl21 . O25 . 109.8(7) yes
O24 . Cl21 . O25 . 111.4(6) yes
O24 5_555 O23 . O25 5_555 115.4(11) yes
O24 5_555 O23 . Cl21 . 60.2(5) yes
O25 5_555 O23 . Cl21 . 60.3(5) yes
O23 5_555 O24 . O25 5_555 121.4(13) yes
O23 5_555 O24 . Cl21 . 61.3(5) yes
O25 5_555 O24 . Cl21 . 62.8(6) yes
O23 5_555 O25 . O24 5_555 122.9(10) yes
O23 5_555 O25 . Cl21 . 62.1(5) yes
O24 5_555 O25 . Cl21 . 63.6(5) yes
O30 5_655 Cl26 . O28 5_655 108.7(8) yes
O30 5_655 Cl26 . O29 5_655 109.0(8) yes
O28 5_655 Cl26 . O29 5_655 110.3(8) yes
O30 5_655 Cl26 . O27 . 108.6(7) yes
O28 5_655 Cl26 . O27 . 110.1(8) yes
O29 5_655 Cl26 . O27 . 110.0(8) yes
O30 5_655 Cl26 . O28 . 57.3(10) yes
O28 5_655 Cl26 . O28 . 139.7(15) yes
O29 5_655 Cl26 . O28 . 54.4(10) yes
O27 . Cl26 . O28 . 110.1(8) yes
O30 5_655 Cl26 . O29 . 57.0(10) yes
O28 5_655 Cl26 . O29 . 54.4(10) yes
O29 5_655 Cl26 . O29 . 140.0(15) yes
O27 . Cl26 . O29 . 110.0(8) yes
O28 . Cl26 . O29 . 110.3(8) yes
O30 5_655 Cl26 . O30 . 142.7(15) yes
O28 5_655 Cl26 . O30 . 57.3(10) yes
O29 5_655 Cl26 . O30 . 57.0(10) yes
O27 . Cl26 . O30 . 108.6(7) yes
O28 . Cl26 . O30 . 108.7(8) yes
O29 . Cl26 . O30 . 109.0(8) yes
O30 5_655 O28 . O29 5_655 121.3(14) yes
O30 5_655 O28 . Cl26 . 61.9(6) yes
O29 5_655 O28 . Cl26 . 62.8(6) yes
O30 5_655 O29 . O28 5_655 121.5(14) yes
O30 5_655 O29 . Cl26 . 62.1(6) yes
O28 5_655 O29 . Cl26 . 62.9(6) yes
O28 5_655 O30 . O29 5_655 117.2(15) yes
O28 5_655 O30 . Cl26 . 60.8(7) yes
O29 5_655 O30 . Cl26 . 60.9(7) yes
Mn2 . N3 . C4 . 122.2(6) yes
Mn2 . N3 . C8 . 117.3(6) yes
C4 . N3 . C8 . 119.9(9) yes
N3 . C4 . C5 . 120.5(9) yes
N3 . C4 . H41 . 119.6 no
C5 . C4 . H41 . 120.0 no
C4 . C5 . C6 . 121.3(10) yes
C4 . C5 . H51 . 119.6 no
C6 . C5 . H51 . 119.0 no
C5 . C6 . C7 . 114.8(14) yes
C5 . C6 . H61 . 122.5 no
C7 . C6 . H61 . 122.7 no
C6 . C7 . C8 . 124.5(11) yes
C6 . C7 . H71 . 117.8 no
C8 . C7 . H71 . 117.7 no
N3 . C8 . C7 . 118.2(8) yes
N3 . C8 . C9 . 116.1(10) yes
C7 . C8 . C9 . 125.6(10) yes
C8 . C9 . C10 . 118.8(10) yes
C8 . C9 . N14 . 117.2(7) yes
C10 . C9 . N14 . 124.0(8) yes
C9 . C10 . C11 . 114.7(9) yes
C9 . C10 . H101 . 123.5 no
C11 . C10 . H101 . 121.8 no
C10 . C11 . C12 . 120.3(8) yes
C10 . C11 . H111 . 119.7 no
C12 . C11 . H111 . 119.9 no
C11 . C12 . C13 . 119.3(9) yes
C11 . C12 . H121 . 120.1 no
C13 . C12 . H121 . 120.6 no
C12 . C13 . N14 . 122.9(9) yes
C12 . C13 . H131 . 118.5 no
N14 . C13 . H131 . 118.5 no
Mn2 . N14 . C9 . 115.1(5) yes
Mn2 . N14 . C13 . 125.6(7) yes
C9 . N14 . C13 . 118.6(7) yes
# Attachment 'mcht02.cif'
data_mcht02
_database_code_depnum_ccdc_archive 'CCDC 730664'
#0.57 GPa data set.
_audit_creation_date 08-12-19
_audit_creation_method CRYSTALS_ver_12.86
_oxford_structure_analysis_title 'mcht02b in I2/m'
_chemical_name_systematic ?
_chemical_melting_point ?
_chemical_compound_source 'Alessandro Prescimone'
_publ_section_exptl_refinement
;
H atoms placed geometrically after each cycle on carbon.
Those attached to O were located from H-bonding considerations
and allowed to ride on their parent O-atoms.
Checkcif output:
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.69
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 12.21 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.73
088_ALERT_3_B Poor Data / Parameter Ratio .................... 6.27
911_ALERT_3_B # Missing FCF Refl Between THmin & STh/L= 0.588 878
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 1
These alerts all derive from shading of reciprocal space by the pressure cell,
and they are unavoidable in high pressure crystal structure determinations.
023_ALERT_3_C Resolution (too) Low [sin(th)/Lambda < 0.6]..... 16.28 Deg.
Rint and Rsigma increase sharply beyond 0.9 Ang. resolution.
INTENSITY STATISTICS FOR DATASET # 1 mcht02.hkl
Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma
Inf - 2.21 121 176 68.8 4.42 154.7 46.71 0.0275 0.0195
2.21 - 1.77 117 158 74.1 3.92 108.5 37.69 0.0273 0.0210
1.77 - 1.55 120 157 76.4 4.02 86.2 30.77 0.0366 0.0248
1.55 - 1.41 123 161 76.4 3.60 60.1 24.98 0.0373 0.0317
1.41 - 1.30 130 173 75.1 3.50 55.4 22.43 0.0446 0.0352
1.30 - 1.22 123 176 69.9 3.34 33.4 16.56 0.0641 0.0494
1.22 - 1.16 118 168 70.2 3.13 21.7 11.42 0.0941 0.0745
1.16 - 1.11 122 167 73.1 3.34 22.6 11.07 0.0966 0.0740
1.11 - 1.06 127 185 68.6 3.03 16.8 9.25 0.1137 0.0990
1.06 - 1.02 140 194 72.2 2.91 15.8 8.14 0.1284 0.1139
1.02 - 0.98 146 221 66.1 2.67 14.1 6.31 0.1690 0.1387
0.98 - 0.95 122 177 68.9 2.62 12.7 6.33 0.1632 0.1497
0.95 - 0.92 141 217 65.0 2.58 8.8 4.66 0.2174 0.2183
0.92 - 0.89 155 240 64.6 2.16 7.6 3.72 0.2324 0.2707
0.89 - 0.86 180 298 60.4 2.34 5.1 2.75 0.3235 0.3873
0.86 - 0.83 177 306 57.8 2.00 4.3 2.01 0.4324 0.5124
0.83 - 0.81 146 254 57.5 1.99 2.8 1.36 0.5241 0.7560
0.81 - 0.80 7 19 36.8 0.63 2.7 0.77 0.7432 1.1769
#-----------------------------------------------------------------------------
0.90 - 0.80 605 1029 58.8 2.08 4.6 2.28 0.3623 0.4577
Inf - 0.80 2315 3447 67.2 2.89 33.8 13.29 0.0586 0.0591
601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 186.00 A**3
In the ambient structure there is presence of 2 half occupied CH3CN
molecules per complex molecule. At high pressure no extra peaks assignable to
solvent are present in the difference map. Forcing the presence of a solvent
molecule in the same position as in the ambient structure doesn't improve the
R-factor and actually refines to an occupancy very close to zero. We should
therefore assume that the solvent has been squeezed out of the crystal as
effect of the high pressure.
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
the reported formula takes in account the solvent molecule that is actually not
present in the crystal anymore.
910_ALERT_3_C # Missing FCF Reflections Below Th(Min) ........ 5
913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 46
Very strong reflections overload the detector pixels with synchrotron
radiation.
420_ALERT_2_B D-H Without Acceptor O20 - H201 ... ?
No suitable acceptors were found at reasonable orientation, the H-atom has been
positioned geometrically.
432_ALERT_2_A Short Inter X...Y Contact O23 .. C4 .. 2.71 Ang.
432_ALERT_2_C Short Inter X...Y Contact C5 .. O29 .. 2.96 Ang.
These are contacts between a disordered Oxygen from a perchlorate and an
aromatic CH group. These contacts can not be avoided.
432_ALERT_2_B Short Inter X...Y Contact O25 .. C16 .. 2.84 Ang.
This is a contact between a disordered Oxygen from a perchlorate and a CH
group from the "cht" ligand. These contacts can not be avoided.
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . CL26
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O27
the occupancy for these atoms is set to be less than 1 despite being on a
special position because in the overall formula there must be 3 perchlorates
to keep the charges balanced. With the occupancy set to 0.5 the R-factor is
lower than the full occupancy case.
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O28
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O29
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O30
These alert is due the program getting confused from the disordered Oxygens
atom on a perchlorate anion: in fact these atoms do not have three covalents
bonds but only one with a Chlorine atom.
128_ALERT_4_C Non-standard setting of Space group C2/m .... I2/m
This setting has been chosen to keep the model of the structure consistent with
ambient pressure structure already present in literature.
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl21
these are quite heavy atoms with an higher coordiantion number compared to
the atoms are attached to: therefore this effect is not surprising.
213_ALERT_2_C Atom C19 has ADP max/min Ratio ............. 3.50 oblate
241_ALERT_2_C Check High Ueq as Compared to Neighbors for O20
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C12
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C8
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for Cl26
302_ALERT_4_C Anion/Solvent Disorder ......................... 34.00 Perc.
341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11
no action here.
;
#end of refcif
_cell_length_a 11.549(2)
_cell_length_b 21.720(4)
_cell_length_c 12.991(3)
_cell_angle_alpha 90
_cell_angle_beta 94.04(3)
_cell_angle_gamma 90
_cell_volume 3250.7(11)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'I 1 2/m 1 '
_symmetry_space_group_name_Hall '-I 2y'
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,-z
x,-y,z
-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 0.0000 0.0010 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'
N 0.0010 0.0010 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 0.0030 0.0030 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'
Cl 0.0750 0.0710 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.2220 0.3450 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C54 H54 Cl3 Mn3 N9 O18
# Dc = 1.42 Fooo = 1380.00 Mu = 7.70 M = 347.05
# Found Formula = C52 H52 Cl3 Mn3 N8 O18
# Dc = 1.38 FOOO = 1380.00 Mu = 7.67 M = 337.04
_chemical_formula_sum 'C52 H52 Cl3 Mn3 N8 O18'
_chemical_formula_moiety '[Mn3(BPy)4(cht)2][ClO4]3'
_chemical_formula_weight 1348.17
_cell_measurement_reflns_used 2203
_cell_measurement_theta_min 2
_cell_measurement_theta_max 15
_cell_measurement_temperature 300
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_min 0.08
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_max 0.11
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1380
_exptl_absorpt_coefficient_mu 0.767
# Sheldrick geometric approximatio 0.93 0.94
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.49
_exptl_absorpt_correction_T_max 0.94
_diffrn_measurement_device 'Bruker SMART APEX-II on Station 9.8, SRS'
_diffrn_measurement_device_type Area
_diffrn_radiation_monochromator silicon
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.47670
_diffrn_measurement_method \w
# 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 ?
_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 300
_diffrn_ambient_pressure 570000
_diffrn_reflns_number 8838
_reflns_number_total 1985
_diffrn_reflns_av_R_equivalents 0.057
# Number of reflections with Friedels Law is 1985
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 2770
_diffrn_reflns_theta_min 1.981
_diffrn_reflns_theta_max 16.285
_diffrn_measured_fraction_theta_max 0.692
_diffrn_reflns_theta_full 12.213
_diffrn_measured_fraction_theta_full 0.731
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 12
_reflns_limit_h_min -13
_reflns_limit_h_max 13
_reflns_limit_k_min -25
_reflns_limit_k_max 25
_reflns_limit_l_min -11
_reflns_limit_l_max 12
_oxford_diffrn_Wilson_B_factor 3.16
_oxford_diffrn_Wilson_scale 5.18
_atom_sites_solution_primary 'From ambient pressure structure'
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.30
_refine_diff_density_max 0.41
# 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>2.0\s(I)
_refine_ls_number_reflns 1223
_refine_ls_number_restraints 31
_refine_ls_number_parameters 195
_oxford_refine_ls_R_factor_ref 0.0665
_refine_ls_wR_factor_ref 0.0398
_refine_ls_goodness_of_fit_ref 0.9624
_refine_ls_shift/su_max 0.002674
# The values computed from all data
_oxford_reflns_number_all 1775
_refine_ls_R_factor_all 0.1031
_refine_ls_wR_factor_all 0.0433
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 1223
_refine_ls_R_factor_gt 0.0665
_refine_ls_wR_factor_gt 0.0398
# 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 sigma
_refine_ls_weighting_details
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;
# 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.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
;
# 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
Mn1 Mn 1.0000 0.5000 0.5000 0.0424 1.0000 Uani S T . . . . .
Mn2 Mn 1.0000 0.64362(4) 0.5000 0.0445 1.0000 Uani S T . . . . .
N3 N 1.1177(3) 0.66179(17) 0.6415(5) 0.0586 1.0000 Uani . . . . . . .
C4 C 1.2136(4) 0.6308(3) 0.6655(7) 0.0754 1.0000 Uani . . . . . . .
C5 C 1.2794(6) 0.6377(4) 0.7547(9) 0.0967 1.0000 Uani . . . . . . .
C6 C 1.2461(7) 0.6760(4) 0.8283(9) 0.0932 1.0000 Uani . . . . . . .
C7 C 1.1376(6) 0.7072(3) 0.8092(7) 0.0928 1.0000 Uani . . . . . . .
C8 C 1.0792(5) 0.7012(2) 0.7138(6) 0.0514 1.0000 Uani . . . . . . .
C9 C 0.9722(5) 0.7343(2) 0.6820(6) 0.0671 1.0000 Uani . . . . . . .
C10 C 0.9341(6) 0.7856(3) 0.7341(7) 0.0830 1.0000 Uani . . . . . . .
C11 C 0.8350(8) 0.8135(3) 0.7037(9) 0.1016 1.0000 Uani . . . . . . .
C12 C 0.7650(8) 0.7892(4) 0.6179(10) 0.1120 1.0000 Uani . . . . . . .
C13 C 0.8096(5) 0.7409(2) 0.5679(6) 0.0816 1.0000 Uani . . . . . . .
N14 N 0.9081(4) 0.71331(17) 0.5981(5) 0.0653 1.0000 Uani . . . . . . .
O15 O 1.0992(2) 0.56504(12) 0.4640(3) 0.0524 1.0000 Uani . . . . . . .
C16 C 1.1804(4) 0.55815(19) 0.3859(7) 0.0607 1.0000 Uani . . . . . . .
C17 C 1.2518(6) 0.500000(6) 0.4058(9) 0.0690 1.0000 Uani S T . . . . .
C18 C 1.1193(6) 0.5577(2) 0.2842(7) 0.0763 1.0000 Uani . . . . . . .
C19 C 1.0452(8) 0.500000(7) 0.2622(8) 0.0623 1.0000 Uani S T . . . . .
O20 O 0.9471(5) 0.500000(7) 0.3256(6) 0.0735 1.0000 Uani S T . . . . .
Cl21 Cl 0.0000 0.13897(7) 0.0000 0.0522 1.0000 Uani DS T . . . . .
O22 O 0.0000 0.2048(2) 0.0000 0.162(2) 1.0000 Uiso DS . . . . . .
O23 O -0.0932(10) 0.1185(5) 0.0600(12) 0.162(2) 0.5000 Uiso D . . . . . .
O24 O -0.0197(13) 0.1143(5) -0.1016(6) 0.162(2) 0.5000 Uiso D . . . . . .
O25 O 0.1075(8) 0.1165(5) 0.0462(13) 0.162(2) 0.5000 Uiso D . . . . . .
Cl26 Cl 0.5000 0.3990(4) 0.0000 0.178(3) 0.5000 Uiso DS . . . . . .
O27 O 0.5000 0.3377(5) 0.0000 0.150(4) 0.5000 Uiso DS . . . . . .
O28 O 0.538(2) 0.4194(7) -0.0887(11) 0.150(4) 0.2500 Uiso D . . . . . .
O29 O 0.569(2) 0.4199(7) 0.0790(14) 0.150(4) 0.2500 Uiso D . . . . . .
O30 O 0.3923(9) 0.4199(7) 0.010(3) 0.150(4) 0.2500 Uiso D . . . . . .
H41 H 1.2403 0.6023 0.6170 0.0500 1.0000 Uiso R . . . . . .
H51 H 1.3492 0.6147 0.7663 0.0500 1.0000 Uiso R . . . . . .
H61 H 1.2937 0.6812 0.8904 0.0500 1.0000 Uiso R . . . . . .
H71 H 1.1065 0.7315 0.8615 0.0500 1.0000 Uiso R . . . . . .
H101 H 0.9760 0.7998 0.7951 0.0500 1.0000 Uiso R . . . . . .
H111 H 0.8124 0.8508 0.7348 0.0500 1.0000 Uiso R . . . . . .
H121 H 0.6908 0.8063 0.5988 0.0500 1.0000 Uiso R . . . . . .
H131 H 0.7650 0.7239 0.5105 0.0500 1.0000 Uiso R . . . . . .
H161 H 1.2304 0.5929 0.3901 0.0500 1.0000 Uiso R . . . . . .
H171 H 1.2802 0.5000 0.4762 0.0500 1.0000 Uiso RS . . . . . .
H172 H 1.3154 0.5000 0.3632 0.0500 1.0000 Uiso RS . . . . . .
H181 H 1.1761 0.5612 0.2350 0.0500 1.0000 Uiso R . . . . . .
H182 H 1.0670 0.5914 0.2766 0.0500 1.0000 Uiso R . . . . . .
H191 H 1.0194 0.5000 0.1911 0.0500 1.0000 Uiso RS . . . . . .
H201 H 0.8733 0.5000 0.2983 0.0500 1.0000 Uiso RS . . . . . .
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
Mn1 0.0477(7) 0.0349(8) 0.0458(18) 0.0000 0.0116(8) 0.0000
Mn2 0.0521(5) 0.0371(6) 0.0440(13) 0.0000 0.0015(6) 0.0000
N3 0.064(2) 0.050(3) 0.062(6) -0.010(2) 0.004(3) -0.0004(19)
C4 0.060(3) 0.068(4) 0.094(9) -0.011(3) -0.025(4) 0.006(3)
C5 0.094(4) 0.087(5) 0.104(12) -0.001(5) -0.026(6) 0.014(4)
C6 0.099(5) 0.123(7) 0.056(11) -0.009(5) -0.013(5) 0.000(4)
C7 0.113(5) 0.094(5) 0.068(10) -0.023(4) -0.022(5) 0.011(4)
C8 0.067(3) 0.062(3) 0.025(7) -0.008(2) 0.005(3) -0.013(2)
C9 0.075(3) 0.046(3) 0.082(8) -0.013(3) 0.018(4) 0.000(3)
C10 0.087(4) 0.079(5) 0.084(10) -0.028(3) 0.015(4) 0.017(3)
C11 0.130(6) 0.089(5) 0.091(11) -0.019(5) 0.042(6) 0.037(5)
C12 0.114(6) 0.117(7) 0.108(13) 0.008(5) 0.032(6) 0.065(5)
C13 0.077(3) 0.058(4) 0.108(10) -0.003(3) -0.002(4) 0.018(3)
N14 0.069(3) 0.047(3) 0.080(7) -0.004(2) 0.008(3) 0.008(2)
O15 0.0540(16) 0.0379(19) 0.067(4) -0.0019(15) 0.0164(19) -0.0031(13)
C16 0.061(3) 0.039(3) 0.086(9) 0.011(2) 0.034(4) 0.0000(19)
C17 0.055(4) 0.064(5) 0.090(12) 0.0000 0.023(5) 0.0000
C18 0.109(4) 0.048(4) 0.075(10) 0.013(3) 0.031(5) -0.001(3)
C19 0.111(6) 0.066(5) 0.011(10) 0.0000 0.014(6) 0.0000
O20 0.068(3) 0.086(4) 0.066(8) 0.0000 0.000(4) 0.0000
Cl21 0.0462(8) 0.0663(11) 0.045(2) 0.0000 0.0096(9) 0.0000
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.5690(19)
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
Mn1 . O20 2_766 2.304(7) yes
Mn1 . O15 6_565 1.898(3) yes
Mn1 . O15 2_766 1.898(3) yes
Mn1 . O15 5_756 1.898(3) yes
Mn1 . O15 . 1.898(3) yes
Mn1 . O20 . 2.304(7) yes
Mn2 . N3 5_756 2.243(5) yes
Mn2 . N14 5_756 2.287(5) yes
Mn2 . O15 5_756 2.126(3) yes
Mn2 . N3 . 2.243(5) yes
Mn2 . N14 . 2.287(5) yes
Mn2 . O15 . 2.126(3) yes
N3 . C4 . 1.315(6) yes
N3 . C8 . 1.367(8) yes
C4 . C5 . 1.349(11) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.344(13) yes
C5 . H51 . 0.950 no
C6 . C7 . 1.431(10) yes
C6 . H61 . 0.950 no
C7 . C8 . 1.375(10) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.464(8) yes
C9 . C10 . 1.393(8) yes
C9 . N14 . 1.354(9) yes
C10 . C11 . 1.329(10) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.430(12) yes
C11 . H111 . 0.950 no
C12 . C13 . 1.356(10) yes
C12 . H121 . 0.950 no
C13 . N14 . 1.320(7) yes
C13 . H131 . 0.950 no
O15 . C16 . 1.438(8) yes
C16 . C17 . 1.521(6) yes
C16 . C18 . 1.453(10) yes
C16 . H161 . 0.950 no
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.533(7) yes
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C19 . O20 . 1.448(11) yes
C19 . H191 . 0.950 no
O20 . H201 . 0.900 no
Cl21 . O23 5_555 1.443(5) yes
Cl21 . O24 5_555 1.428(7) yes
Cl21 . O25 5_555 1.427(6) yes
Cl21 . O22 . 1.431(5) yes
Cl21 . O23 . 1.443(5) yes
Cl21 . O24 . 1.428(7) yes
Cl21 . O25 . 1.427(6) yes
O23 . O25 5_555 1.379(16) yes
O23 . O24 5_555 1.379(11) yes
O24 . O25 5_555 1.286(14) yes
Cl26 . O30 5_655 1.338(7) yes
Cl26 . O29 5_655 1.336(6) yes
Cl26 . O28 5_655 1.335(6) yes
Cl26 . O27 . 1.331(8) yes
Cl26 . O28 . 1.335(6) yes
Cl26 . O29 . 1.336(6) yes
Cl26 . O30 . 1.338(7) yes
O28 . O30 5_655 1.260(19) yes
O28 . O29 5_655 1.249(18) yes
O29 . O30 5_655 1.266(19) 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
O20 2_766 Mn1 . O15 6_565 96.87(15) yes
O20 2_766 Mn1 . O15 2_766 83.13(15) yes
O15 6_565 Mn1 . O15 2_766 83.79(17) yes
O20 2_766 Mn1 . O15 5_756 83.13(15) yes
O15 6_565 Mn1 . O15 5_756 179.994 yes
O15 2_766 Mn1 . O15 5_756 96.21(17) yes
O20 2_766 Mn1 . O15 . 96.87(15) yes
O15 6_565 Mn1 . O15 . 96.21(17) yes
O15 2_766 Mn1 . O15 . 179.994 yes
O15 5_756 Mn1 . O15 . 83.79(17) yes
O20 2_766 Mn1 . O20 . 179.995 yes
O15 6_565 Mn1 . O20 . 83.13(15) yes
O15 2_766 Mn1 . O20 . 96.87(15) yes
O15 5_756 Mn1 . O20 . 96.87(15) yes
O15 . Mn1 . O20 . 83.13(15) yes
N3 5_756 Mn2 . N14 5_756 72.85(18) yes
N3 5_756 Mn2 . O15 5_756 90.98(14) yes
N14 5_756 Mn2 . O15 5_756 158.80(19) yes
N3 5_756 Mn2 . N3 . 159.7(2) yes
N14 5_756 Mn2 . N3 . 93.6(2) yes
O15 5_756 Mn2 . N3 . 105.39(16) yes
N3 5_756 Mn2 . N14 . 93.6(2) yes
N14 5_756 Mn2 . N14 . 97.1(2) yes
O15 5_756 Mn2 . N14 . 97.49(15) yes
N3 . Mn2 . N14 . 72.85(18) yes
N3 5_756 Mn2 . O15 . 105.39(16) yes
N14 5_756 Mn2 . O15 . 97.49(15) yes
O15 5_756 Mn2 . O15 . 73.19(16) yes
N3 . Mn2 . O15 . 90.98(14) yes
N14 . Mn2 . O15 . 158.80(19) yes
Mn2 . N3 . C4 . 123.7(4) yes
Mn2 . N3 . C8 . 117.8(4) yes
C4 . N3 . C8 . 117.8(6) yes
N3 . C4 . C5 . 124.1(7) yes
N3 . C4 . H41 . 119.0 no
C5 . C4 . H41 . 116.9 no
C4 . C5 . C6 . 120.5(7) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 119.7 no
C5 . C6 . C7 . 117.4(9) yes
C5 . C6 . H61 . 119.9 no
C7 . C6 . H61 . 122.6 no
C6 . C7 . C8 . 118.6(7) yes
C6 . C7 . H71 . 120.6 no
C8 . C7 . H71 . 120.8 no
C7 . C8 . N3 . 121.1(5) yes
C7 . C8 . C9 . 123.9(6) yes
N3 . C8 . C9 . 115.0(6) yes
C8 . C9 . C10 . 123.1(7) yes
C8 . C9 . N14 . 117.7(5) yes
C10 . C9 . N14 . 119.2(5) yes
C9 . C10 . C11 . 121.0(7) yes
C9 . C10 . H101 . 120.3 no
C11 . C10 . H101 . 118.5 no
C10 . C11 . C12 . 119.5(6) yes
C10 . C11 . H111 . 121.2 no
C12 . C11 . H111 . 119.2 no
C11 . C12 . C13 . 116.4(7) yes
C11 . C12 . H121 . 120.7 no
C13 . C12 . H121 . 122.9 no
C12 . C13 . N14 . 123.9(8) yes
C12 . C13 . H131 . 118.2 no
N14 . C13 . H131 . 117.7 no
Mn2 . N14 . C9 . 115.0(3) yes
Mn2 . N14 . C13 . 124.0(5) yes
C9 . N14 . C13 . 119.8(5) yes
Mn2 . O15 . Mn1 . 101.51(13) yes
Mn2 . O15 . C16 . 128.9(3) yes
Mn1 . O15 . C16 . 122.1(3) yes
O15 . C16 . C17 . 109.9(6) yes
O15 . C16 . C18 . 110.1(5) yes
C17 . C16 . C18 . 111.8(6) yes
O15 . C16 . H161 . 107.5 no
C17 . C16 . H161 . 109.3 no
C18 . C16 . H161 . 108.1 no
C16 . C17 . C16 6_565 112.3(6) yes
C16 . C17 . H171 . 108.0 no
C16 6_565 C17 . H171 . 108.0 no
C16 . C17 . H172 . 109.5 no
C16 6_565 C17 . H172 . 109.5 no
H171 . C17 . H172 . 109.5 no
C16 . C18 . C19 . 113.8(5) yes
C16 . C18 . H181 . 107.3 no
C19 . C18 . H181 . 110.0 no
C16 . C18 . H182 . 110.7 no
C19 . C18 . H182 . 105.5 no
H181 . C18 . H182 . 109.5 no
C18 6_565 C19 . C18 . 109.7(7) yes
C18 6_565 C19 . O20 . 110.1(5) yes
C18 . C19 . O20 . 110.1(5) yes
C18 6_565 C19 . H191 . 108.3 no
C18 . C19 . H191 . 108.3 no
O20 . C19 . H191 . 110.4 no
C19 . O20 . Mn1 . 113.3(5) yes
C19 . O20 . H201 . 122.2 no
Mn1 . O20 . H201 . 124.5 no
O23 5_555 Cl21 . O24 5_555 107.9(5) yes
O23 5_555 Cl21 . O25 5_555 109.1(6) yes
O24 5_555 Cl21 . O25 5_555 109.7(5) yes
O23 5_555 Cl21 . O22 . 108.0(4) yes
O24 5_555 Cl21 . O22 . 112.0(5) yes
O25 5_555 Cl21 . O22 . 110.0(4) yes
O23 5_555 Cl21 . O23 . 144.1(8) yes
O24 5_555 Cl21 . O23 . 57.4(5) yes
O25 5_555 Cl21 . O23 . 57.4(6) yes
O22 . Cl21 . O23 . 108.0(4) yes
O23 5_555 Cl21 . O24 . 57.4(5) yes
O24 5_555 Cl21 . O24 . 135.9(10) yes
O25 5_555 Cl21 . O24 . 53.5(6) yes
O22 . Cl21 . O24 . 112.0(5) yes
O23 . Cl21 . O24 . 107.9(5) yes
O23 5_555 Cl21 . O25 . 57.4(6) yes
O24 5_555 Cl21 . O25 . 53.5(6) yes
O25 5_555 Cl21 . O25 . 140.0(9) yes
O22 . Cl21 . O25 . 110.0(4) yes
O23 . Cl21 . O25 . 109.1(6) yes
O24 . Cl21 . O25 . 109.7(5) yes
O25 5_555 O23 . O24 5_555 115.7(8) yes
O25 5_555 O23 . Cl21 . 60.7(4) yes
O24 5_555 O23 . Cl21 . 60.7(4) yes
O23 5_555 O24 . O25 5_555 122.7(10) yes
O23 5_555 O24 . Cl21 . 61.9(4) yes
O25 5_555 O24 . Cl21 . 63.2(5) yes
O23 5_555 O25 . O24 5_555 121.2(8) yes
O23 5_555 O25 . Cl21 . 61.9(4) yes
O24 5_555 O25 . Cl21 . 63.3(4) yes
O30 5_655 Cl26 . O29 5_655 108.8(7) yes
O30 5_655 Cl26 . O28 5_655 109.3(7) yes
O29 5_655 Cl26 . O28 5_655 109.7(7) yes
O30 5_655 Cl26 . O27 . 109.8(7) yes
O29 5_655 Cl26 . O27 . 109.8(7) yes
O28 5_655 Cl26 . O27 . 109.4(7) yes
O30 5_655 Cl26 . O28 . 56.2(8) yes
O29 5_655 Cl26 . O28 . 55.7(8) yes
O28 5_655 Cl26 . O28 . 141.1(14) yes
O27 . Cl26 . O28 . 109.4(7) yes
O30 5_655 Cl26 . O29 . 56.5(9) yes
O29 5_655 Cl26 . O29 . 140.3(14) yes
O28 5_655 Cl26 . O29 . 55.7(8) yes
O27 . Cl26 . O29 . 109.8(7) yes
O28 . Cl26 . O29 . 109.7(7) yes
O30 5_655 Cl26 . O30 . 140.3(13) yes
O29 5_655 Cl26 . O30 . 56.5(9) yes
O28 5_655 Cl26 . O30 . 56.2(8) yes
O27 . Cl26 . O30 . 109.8(7) yes
O28 . Cl26 . O30 . 109.3(7) yes
O29 . Cl26 . O30 . 108.8(7) yes
O30 5_655 O28 . O29 5_655 120.1(13) yes
O30 5_655 O28 . Cl26 . 62.0(6) yes
O29 5_655 O28 . Cl26 . 62.1(6) yes
O30 5_655 O29 . O28 5_655 120.2(12) yes
O30 5_655 O29 . Cl26 . 61.9(6) yes
O28 5_655 O29 . Cl26 . 62.1(5) yes
O29 5_655 O30 . O28 5_655 119.7(12) yes
O29 5_655 O30 . Cl26 . 61.6(6) yes
O28 5_655 O30 . Cl26 . 61.8(6) yes
# Attachment 'mcht03.cif'
data_mcht03
_database_code_depnum_ccdc_archive 'CCDC 730665'
#1.25 GPa data set.
_audit_creation_date 08-12-22
_audit_creation_method CRYSTALS_ver_12.86
_oxford_structure_analysis_title 'mcht03b in I2/m'
_chemical_name_systematic ?
_chemical_melting_point ?
_chemical_compound_source 'Alessandro Prescimone'
_publ_section_exptl_refinement
;
H atoms placed geometrically after each cycle on carbon.
Those attached to C atoms on the aromatic rings are part of
the rigid body.
Each aromatic ring has been refined as rigid body.
Perchlorates have been constrained to be tetrahedric
Checkcif output:
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.70
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 11.51 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.74
201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 18
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 1
These alerts all derive from shading of reciprocal space by the pressure cell,
and they are unavoidable in high pressure crystal structure determinations.
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 15.35 Deg.
Rint and Rsigma increase sharply beyond 0.9 Ang. resolution.
INTENSITY STATISTICS FOR DATASET # 1 mcht03.hkl
Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma
Inf - 2.25 113 157 72.0 4.15 131.0 37.09 0.0287 0.0212
2.25 - 1.79 119 154 77.3 3.31 67.1 25.91 0.0372 0.0303
1.79 - 1.56 115 154 74.7 2.95 46.3 19.19 0.0504 0.0423
1.56 - 1.41 119 159 74.8 2.96 37.5 16.16 0.0538 0.0509
1.41 - 1.31 119 162 73.5 2.91 31.9 13.61 0.0711 0.0610
1.31 - 1.23 112 160 70.0 2.69 18.9 9.59 0.1173 0.0997
1.23 - 1.16 123 170 72.4 2.73 12.8 6.56 0.1386 0.1450
1.16 - 1.11 125 167 74.9 2.83 13.9 6.34 0.1704 0.1504
1.11 - 1.06 122 183 66.7 2.52 8.7 4.42 0.1984 0.2261
1.06 - 1.02 121 182 66.5 2.35 9.0 4.00 0.2404 0.2423
1.02 - 0.98 142 210 67.6 2.46 7.9 3.52 0.2735 0.2843
0.98 - 0.95 115 179 64.2 2.09 7.4 3.12 0.2775 0.3138
0.95 - 0.92 138 212 65.1 2.17 4.2 1.85 0.4201 0.5695
0.92 - 0.89 147 233 63.1 1.98 4.4 1.93 0.4338 0.5680
0.89 - 0.86 159 265 60.0 1.94 3.3 1.35 0.5440 0.7795
0.86 - 0.84 128 210 61.0 1.80 3.0 1.11 0.5925 0.9446
0.84 - 0.82 112 210 53.3 1.63 2.0 0.80 0.7146 1.3539
0.82 - 0.80 81 149 54.4 1.32 2.0 0.66 0.7532 1.6024
#-----------------------------------------------------------------------------
0.90 - 0.80 583 1001 58.2 1.74 2.9 1.14 0.5751 0.9443
Inf - 0.80 2210 3316 66.6 2.43 21.9 8.42 0.0814 0.1048
601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 172.00 A**3
In the ambient structure there is presence of 2 half occupied CH3CN
molecules per complex molecule. At high pressure no extra peaks assignable to
solvent are present in the difference map. Forcing the presence of a solvent
molecule in the same position as in the ambient structure doesn't improve the
R-factor and actually refines to an occupancy very close to zero. We should
therefore assume that the solvent has been squeezed out of the crystal as
effect of the high pressure.
420_ALERT_2_B D-H Without Acceptor O20 - H201 ... ?
No suitable acceptors were found at reasonable orientation, the H-atom has been
positioned geometrically.
432_ALERT_2_A Short Inter X...Y Contact O23 .. C4 .. 2.61 Ang.
432_ALERT_2_B Short Inter X...Y Contact C5 .. O29 .. 2.80 Ang.
These are contacts between a disordered Oxygen from a perchlorate and an
aromatic CH group. These contacts can not be avoided.
432_ALERT_2_B Short Inter X...Y Contact O25 .. C16 .. 2.80 Ang.
432_ALERT_2_C Short Inter X...Y Contact O25 .. C17 .. 3.00 Ang.
These are contacts between a disordered Oxygen from a perchlorate and CHs
group from the "cht" ligand. These contacts can not be avoided.
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O28
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O29
313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O30
These alert is due the program getting confused from the disordered Oxygens
atom on a perchlorate anion: in fact these atoms do not have three covalents
bonds but only one with a Chlorine atom.
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn1
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Mn2
these are quite heavy atoms with an higher coordiantion number compared to
the atoms are attached to: therefore this effect is not surprising.
341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 11
241_ALERT_2_A Check High Ueq as Compared to Neighbors for C19
795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C9
797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N3
302_ALERT_4_G Anion/Solvent Disorder ......................... 34.00 Perc.
793_ALERT_4_G Check the Absolute Configuration of C16 ..... R
243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for Cl26
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl21
no action here.
731_ALERT_1_A Bond Calc 1.476(9), Rep 1.4763(4) ...... 9.90 su-Ra
C7 -C8 1.555 1.555
732_ALERT_1_A Angle Calc 122.1(5), Rep 122.07(1) ...... 9.90 su-Ra
C10 -C9 -N14 1.555 1.555 1.555
....plus several others alerts of the same kind.
The use of restraints in the refinement mean that off diagonal terms in the
variance-covariance matrix are significant, and the diagonal approximation
used in Platon/Checkcif can be badly in error.
128_ALERT_4_C Non-standard setting of Space group C2/m .... I2/m
This setting has been chosen to keep the model of the structure consistent with
ambient pressure structure already present in literature.
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . CL26
076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O27
the occupancy for these atoms is set to be less than 1 despite being on a
special position because in the overall formula there must be 3 perchlorates
to keep the charges balanced. With the occupancy set to 0.5 the R-factor is
lower than the full occupancy case.
042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
the reported formula takes in account the solvent molecule that is actually not
present in the crystal anymore.
;
#end of refcif
_cell_length_a 11.331(2)
_cell_length_b 21.547(4)
_cell_length_c 12.817(3)
_cell_angle_alpha 90
_cell_angle_beta 93.67(3)
_cell_angle_gamma 90
_cell_volume 3122.9(11)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'I 1 2/m 1 '
_symmetry_space_group_name_Hall '-I 2y'
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,-z
x,-y,z
-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 0.0000 0.0010 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'
N 0.0010 0.0010 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 0.0030 0.0030 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'
Cl 0.0750 0.0710 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Mn 0.2220 0.3450 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543
1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C54 H54 Cl3 Mn3 N9 O18
# Dc = 1.48 Fooo = 1380.00 Mu = 8.01 M = 347.05
# Found Formula = C52 H52 Cl3 Mn3 N8 O18
# Dc = 1.43 FOOO = 1380.00 Mu = 7.98 M = 337.04
_chemical_formula_sum 'C52 H52 Cl3 Mn3 N8 O18'
_chemical_formula_moiety '[Mn3(BPy)4(cht)2][ClO4]3'
_chemical_formula_weight 1348.17
_cell_measurement_reflns_used 1592
_cell_measurement_theta_min 2
_cell_measurement_theta_max 16
_cell_measurement_temperature 300
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_min 0.08
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_max 0.11
_exptl_crystal_density_diffrn 1.434
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1380
_exptl_absorpt_coefficient_mu 0.798
# Sheldrick geometric approximatio 0.92 0.94
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.26
_exptl_absorpt_correction_T_max 0.94
_diffrn_measurement_device 'Bruker SMART APEX-II on Station 9.8, SRS'
_diffrn_measurement_device_type Area
_diffrn_radiation_monochromator silicon
_diffrn_radiation_type Synchrotron
_diffrn_radiation_wavelength 0.47670
_diffrn_measurement_method \w
# 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 ?
_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 300
_diffrn_ambient_pressure 1250000
_diffrn_reflns_number 6315
_reflns_number_total 1627
_diffrn_reflns_av_R_equivalents 0.075
# Number of reflections with Friedels Law is 1627
# Number of reflections without Friedels Law is 0
# Theoretical number of reflections is about 2241
_diffrn_reflns_theta_min 1.268
_diffrn_reflns_theta_max 15.353
_diffrn_measured_fraction_theta_max 0.703
_diffrn_reflns_theta_full 11.514
_diffrn_measured_fraction_theta_full 0.740
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -12
_reflns_limit_h_max 12
_reflns_limit_k_min -23
_reflns_limit_k_max 23
_reflns_limit_l_min -11
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 3.13
_oxford_diffrn_Wilson_scale 8.81
_atom_sites_solution_primary 'From ambient pressure structure'
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.66
_refine_diff_density_max 0.51
# 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>2.0\s(I)
_refine_ls_number_reflns 830
_refine_ls_number_restraints 34
_refine_ls_number_parameters 77
_oxford_refine_ls_R_factor_ref 0.0996
_refine_ls_wR_factor_ref 0.0521
_refine_ls_goodness_of_fit_ref 0.9988
_refine_ls_shift/su_max 0.003004
# The values computed from all data
_oxford_reflns_number_all 1412
_refine_ls_R_factor_all 0.1678
_refine_ls_wR_factor_all 0.0604
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 830
_refine_ls_R_factor_gt 0.0996
_refine_ls_wR_factor_gt 0.0521
# 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 mixed # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details
;
Method=
SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6)
;
# 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.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
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.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
;
# 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
Mn1 Mn 1.0000 0.5000 0.5000 0.0377 1.0000 Uani S T . . . . .
Mn2 Mn 1.0000 0.64469(7) 0.5000 0.0365 1.0000 Uani S T . . . . .
O15 O 1.0990(4) 0.5637(2) 0.4620(5) 0.0432(15) 1.0000 Uiso . . . . . . .
C16 C 1.1835(8) 0.5594(4) 0.3885(11) 0.067(3) 1.0000 Uiso D . . . . . .
C17 C 1.2570(11) 0.500000(6) 0.4079(14) 0.063(4) 1.0000 Uiso S . . . . . .
C18 C 1.1225(10) 0.5588(4) 0.2843(12) 0.092(4) 1.0000 Uiso D . . . . . .
C19 C 1.0536(17) 0.500000(7) 0.269(3) 0.140(7) 1.0000 Uiso DS . . . . . .
O20 O 0.9423(8) 0.500000(7) 0.3234(9) 0.082(3) 1.0000 Uiso S . . . . . .
Cl21 Cl 0.0000 0.13572(13) 0.0000 0.0514 1.0000 Uani DS T . . . . .
O22 O 0.0000 0.1983(3) 0.0000 0.148(3) 1.0000 Uiso DS . . . . . .
O23 O -0.0923(17) 0.1172(6) 0.055(2) 0.148(3) 0.5000 Uiso D . . . . . .
O24 O -0.014(2) 0.1137(6) -0.0972(8) 0.148(3) 0.5000 Uiso D . . . . . .
O25 O 0.1013(14) 0.1156(6) 0.048(2) 0.148(3) 0.5000 Uiso D . . . . . .
Cl26 Cl 0.5000 0.4011(7) 0.0000 0.232(7) 0.5000 Uiso DS . . . . . .
O27 O 0.5000 0.3359(6) 0.0000 0.115(6) 0.5000 Uiso DS . . . . . .
O28 O 0.547(3) 0.4216(9) -0.0940(14) 0.115(6) 0.2500 Uiso D . . . . . .
O29 O 0.573(3) 0.4233(9) 0.0851(17) 0.115(6) 0.2500 Uiso D . . . . . .
O30 O 0.3848(10) 0.4241(8) 0.005(3) 0.115(6) 0.2500 Uiso D . . . . . .
C9 C 0.9685(4) 0.7361(3) 0.6815(6) 0.0761(13) 1.0000 Uiso G . . . . . .
C10 C 0.9350(6) 0.7867(3) 0.7355(5) 0.0761(13) 1.0000 Uiso G . . . . . .
C11 C 0.8368(6) 0.8146(2) 0.7063(6) 0.0761(13) 1.0000 Uiso G . . . . . .
C12 C 0.7654(4) 0.7910(3) 0.6305(6) 0.0761(13) 1.0000 Uiso G . . . . . .
C13 C 0.8010(5) 0.7415(3) 0.5719(5) 0.0761(13) 1.0000 Uiso G . . . . . .
N14 N 0.9051(5) 0.7151(2) 0.5963(5) 0.0734(13) 1.0000 Uiso G . . . . . .
N3 N 1.1206(5) 0.6632(3) 0.6410(4) 0.0720(13) 1.0000 Uiso G . . . . . .
C4 C 1.2169(5) 0.6334(2) 0.6557(5) 0.0720(13) 1.0000 Uiso DG . . . . . .
C5 C 1.2813(4) 0.6364(2) 0.7616(6) 0.0720(13) 1.0000 Uiso DG . . . . . .
C6 C 1.2431(5) 0.6769(3) 0.8349(4) 0.0720(13) 1.0000 Uiso G . . . . . .
C7 C 1.1389(5) 0.7165(3) 0.8127(5) 0.0720(13) 1.0000 Uiso G . . . . . .
C8 C 1.0739(4) 0.7048(2) 0.7111(5) 0.0720(13) 1.0000 Uiso G . . . . . .
H161 H 1.2329 0.5950 0.3944 0.0986 1.0000 Uiso R . . . . . .
H171 H 1.3260 0.5000 0.3696 0.0809 1.0000 Uiso RS . . . . . .
H172 H 1.2790 0.5000 0.4807 0.0809 1.0000 Uiso RS . . . . . .
H181 H 1.1784 0.5645 0.2330 0.1269 1.0000 Uiso R . . . . . .
H182 H 1.0674 0.5920 0.2806 0.1269 1.0000 Uiso R . . . . . .
H191 H 1.0292 0.5000 0.1969 0.1857 1.0000 Uiso RS . . . . . .
H101 H 0.9831 0.8027 0.7922 0.0912 1.0000 Uiso . . . . . . .
H111 H 0.8156 0.8528 0.7382 0.0912 1.0000 Uiso . . . . . . .
H121 H 0.6879 0.8081 0.6165 0.0912 1.0000 Uiso . . . . . . .
H131 H 0.7500 0.7255 0.5161 0.0912 1.0000 Uiso . . . . . . .
H41 H 1.2475 0.6100 0.6003 0.0839 1.0000 Uiso . . . . . . .
H51 H 1.3492 0.6106 0.7765 0.0839 1.0000 Uiso . . . . . . .
H61 H 1.2876 0.6796 0.9007 0.0839 1.0000 Uiso . . . . . . .
H71 H 1.1178 0.7474 0.8606 0.0839 1.0000 Uiso . . . . . . .
H201 H 0.8670 0.5000 0.2964 0.0887 1.0000 Uiso RS . . . . . .
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
Mn1 0.0506(15) 0.0330(16) 0.032(3) 0.0000 0.0178(16) 0.0000
Mn2 0.0462(10) 0.0303(11) 0.033(2) 0.0000 0.0025(11) 0.0000
Cl21 0.0466(16) 0.055(2) 0.055(5) 0.0000 0.021(2) 0.0000
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.4082(17)
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
Mn1 . O20 2_766 2.315(12) yes
Mn1 . O15 6_565 1.858(5) yes
Mn1 . O15 5_756 1.858(5) yes
Mn1 . O15 2_766 1.858(5) yes
Mn1 . O15 . 1.858(5) yes
Mn1 . O20 . 2.315(12) yes
Mn2 . N3 5_756 2.231(5) yes
Mn2 . N14 5_756 2.269(5) yes
Mn2 . O15 5_756 2.147(5) yes
Mn2 . O15 . 2.147(5) yes
Mn2 . N14 . 2.269(5) yes
Mn2 . N3 . 2.231(5) yes
O15 . C16 . 1.388(12) yes
C16 . C17 . 1.538(10) yes
C16 . C18 . 1.464(9) yes
C16 . H161 . 0.950 no
C17 . H171 . 0.950 no
C17 . H172 . 0.950 no
C18 . C19 . 1.494(8) yes
C18 . H181 . 0.950 no
C18 . H182 . 0.950 no
C19 . O20 . 1.48(2) yes
C19 . H191 . 0.950 no
O20 . H201 . 0.900 no
Cl21 . O23 5_555 1.357(6) yes
Cl21 . O25 5_555 1.339(7) yes
Cl21 . O24 5_555 1.333(7) yes
Cl21 . O22 . 1.349(6) yes
Cl21 . O23 . 1.357(6) yes
Cl21 . O24 . 1.333(7) yes
Cl21 . O25 . 1.339(7) yes
O23 . O25 5_555 1.315(19) yes
O23 . O24 5_555 1.292(16) yes
O24 . O25 5_555 1.208(17) yes
Cl26 . O28 5_655 1.418(6) yes
Cl26 . O29 5_655 1.408(6) yes
Cl26 . O30 5_655 1.401(8) yes
Cl26 . O27 . 1.406(8) yes
Cl26 . O28 . 1.418(6) yes
Cl26 . O29 . 1.408(6) yes
Cl26 . O30 . 1.401(8) yes
O28 . O29 5_655 1.37(2) yes
O28 . O30 5_655 1.34(2) yes
O29 . O30 5_655 1.28(2) yes
C9 . C10 . 1.3588(2) yes
C9 . N14 . 1.3453(4) yes
C9 . C8 . 1.402(6) yes
C10 . C11 . 1.2983(3) yes
C10 . H101 . 0.946 no
C11 . C12 . 1.3259(4) yes
C11 . H111 . 0.955 no
C12 . C13 . 1.3800(2) yes
C12 . H121 . 0.959 no
C13 . N14 . 1.3293(3) yes
C13 . H131 . 0.954 no
N3 . C4 . 1.2704(2) yes
N3 . C8 . 1.3966(2) yes
C4 . C5 . 1.5006(4) yes
C4 . H41 . 0.954 no
C5 . C6 . 1.3733(2) yes
C5 . H51 . 0.959 no
C6 . C7 . 1.4684(2) yes
C6 . H61 . 0.956 no
C7 . C8 . 1.4763(4) yes
C7 . H71 . 0.948 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
O20 2_766 Mn1 . O15 6_565 96.8(2) yes
O20 2_766 Mn1 . O15 5_756 83.2(2) yes
O15 6_565 Mn1 . O15 5_756 179.994 yes
O20 2_766 Mn1 . O15 2_766 83.2(2) yes
O15 6_565 Mn1 . O15 2_766 84.7(3) yes
O15 5_756 Mn1 . O15 2_766 95.3(3) yes
O20 2_766 Mn1 . O15 . 96.8(2) yes
O15 6_565 Mn1 . O15 . 95.3(3) yes
O15 5_756 Mn1 . O15 . 84.7(3) yes
O15 2_766 Mn1 . O15 . 179.994 yes
O20 2_766 Mn1 . O20 . 179.995 yes
O15 6_565 Mn1 . O20 . 83.2(2) yes
O15 5_756 Mn1 . O20 . 96.8(2) yes
O15 2_766 Mn1 . O20 . 96.8(2) yes
O15 . Mn1 . O20 . 83.2(2) yes
N3 5_756 Mn2 . N14 5_756 74.1(2) yes
N3 5_756 Mn2 . O15 5_756 91.6(2) yes
N14 5_756 Mn2 . O15 5_756 159.9(2) yes
N3 5_756 Mn2 . O15 . 105.3(2) yes
N14 5_756 Mn2 . O15 . 98.4(2) yes
O15 5_756 Mn2 . O15 . 71.3(3) yes
N3 5_756 Mn2 . N14 . 92.0(2) yes
N14 5_756 Mn2 . N14 . 96.1(3) yes
O15 5_756 Mn2 . N14 . 98.4(2) yes
O15 . Mn2 . N14 . 159.9(2) yes
N3 5_756 Mn2 . N3 . 159.4(3) yes
N14 5_756 Mn2 . N3 . 92.0(2) yes
O15 5_756 Mn2 . N3 . 105.3(2) yes
O15 . Mn2 . N3 . 91.6(2) yes
N14 . Mn2 . N3 . 74.1(2) yes
Mn2 . O15 . Mn1 . 102.0(2) yes
Mn2 . O15 . C16 . 127.0(5) yes
Mn1 . O15 . C16 . 125.6(5) yes
O15 . C16 . C17 . 109.6(9) yes
O15 . C16 . C18 . 108.3(8) yes
C17 . C16 . C18 . 111.0(9) yes
O15 . C16 . H161 . 108.7 no
C17 . C16 . H161 . 110.5 no
C18 . C16 . H161 . 108.7 no
C16 . C17 . C16 6_565 112.6(10) yes
C16 . C17 . H171 . 111.8 no
C16 6_565 C17 . H171 . 111.8 no
C16 . C17 . H172 . 105.3 no
C16 6_565 C17 . H172 . 105.3 no
H171 . C17 . H172 . 109.5 no
C16 . C18 . C19 . 109.8(13) yes
C16 . C18 . H181 . 109.5 no
C19 . C18 . H181 . 112.7 no
C16 . C18 . H182 . 108.0 no
C19 . C18 . H182 . 107.3 no
H181 . C18 . H182 . 109.5 no
C18 . C19 . C18 6_565 115.9(13) yes
C18 . C19 . O20 . 113.2(12) yes
C18 6_565 C19 . O20 . 113.2(12) yes
C18 . C19 . H191 . 104.1 no
C18 6_565 C19 . H191 . 104.1 no
O20 . C19 . H191 . 104.8 no
C19 . O20 . Mn1 . 105.3(12) yes
C19 . O20 . H201 . 129.4 no
Mn1 . O20 . H201 . 125.3 no
O23 5_555 Cl21 . O25 5_555 109.5(7) yes
O23 5_555 Cl21 . O24 5_555 109.3(6) yes
O25 5_555 Cl21 . O24 5_555 111.2(6) yes
O23 5_555 Cl21 . O22 . 107.1(5) yes
O25 5_555 Cl21 . O22 . 108.9(6) yes
O24 5_555 Cl21 . O22 . 110.8(6) yes
O23 5_555 Cl21 . O23 . 145.8(11) yes
O25 5_555 Cl21 . O23 . 58.4(8) yes
O24 5_555 Cl21 . O23 . 57.4(7) yes
O22 . Cl21 . O23 . 107.1(5) yes
O23 5_555 Cl21 . O24 . 57.4(7) yes
O25 5_555 Cl21 . O24 . 53.7(7) yes
O24 5_555 Cl21 . O24 . 138.4(13) yes
O22 . Cl21 . O24 . 110.8(6) yes
O23 . Cl21 . O24 . 109.3(6) yes
O23 5_555 Cl21 . O25 . 58.4(8) yes
O25 5_555 Cl21 . O25 . 142.2(12) yes
O24 5_555 Cl21 . O25 . 53.7(7) yes
O22 . Cl21 . O25 . 108.9(6) yes
O23 . Cl21 . O25 . 109.5(7) yes
O24 . Cl21 . O25 . 111.2(6) yes
O25 5_555 O23 . O24 5_555 115.5(11) yes
O25 5_555 O23 . Cl21 . 60.1(5) yes
O24 5_555 O23 . Cl21 . 60.4(5) yes
O23 5_555 O24 . O25 5_555 123.4(13) yes
O23 5_555 O24 . Cl21 . 62.2(6) yes
O25 5_555 O24 . Cl21 . 63.4(6) yes
O23 5_555 O25 . O24 5_555 120.8(12) yes
O23 5_555 O25 . Cl21 . 61.5(6) yes
O24 5_555 O25 . Cl21 . 62.9(6) yes
O28 5_655 Cl26 . O29 5_655 108.7(7) yes
O28 5_655 Cl26 . O30 5_655 109.1(7) yes
O29 5_655 Cl26 . O30 5_655 110.3(7) yes
O28 5_655 Cl26 . O27 . 108.1(7) yes
O29 5_655 Cl26 . O27 . 109.9(7) yes
O30 5_655 Cl26 . O27 . 110.7(7) yes
O28 5_655 Cl26 . O28 . 143.7(14) yes
O29 5_655 Cl26 . O28 . 57.8(9) yes
O30 5_655 Cl26 . O28 . 56.9(9) yes
O27 . Cl26 . O28 . 108.1(7) yes
O28 5_655 Cl26 . O29 . 57.8(9) yes
O29 5_655 Cl26 . O29 . 140.3(14) yes
O30 5_655 Cl26 . O29 . 54.0(9) yes
O27 . Cl26 . O29 . 109.9(7) yes
O28 . Cl26 . O29 . 108.7(7) yes
O28 5_655 Cl26 . O30 . 56.9(9) yes
O29 5_655 Cl26 . O30 . 54.0(9) yes
O30 5_655 Cl26 . O30 . 138.6(14) yes
O27 . Cl26 . O30 . 110.7(7) yes
O28 . Cl26 . O30 . 109.1(7) yes
O29 . Cl26 . O30 . 110.3(7) yes
O29 5_655 O28 . O30 5_655 116.6(13) yes
O29 5_655 O28 . Cl26 . 60.7(6) yes
O30 5_655 O28 . Cl26 . 60.9(6) yes
O28 5_655 O29 . O30 5_655 120.6(13) yes
O28 5_655 O29 . Cl26 . 61.5(6) yes
O30 5_655 O29 . Cl26 . 62.7(6) yes
O28 5_655 O30 . O29 5_655 122.6(13) yes
O28 5_655 O30 . Cl26 . 62.2(6) yes
O29 5_655 O30 . Cl26 . 63.3(6) yes
C10 . C9 . N14 . 122.075(11) yes
C10 . C9 . C8 . 120.6(6) yes
N14 . C9 . C8 . 117.3(6) yes
C9 . C10 . C11 . 119.190(12) yes
C9 . C10 . H101 . 121.2 no
C11 . C10 . H101 . 119.5 no
C10 . C11 . C12 . 120.31(2) yes
C10 . C11 . H111 . 120.7 no
C12 . C11 . H111 . 119.0 no
C11 . C12 . C13 . 120.638(16) yes
C11 . C12 . H121 . 119.9 no
C13 . C12 . H121 . 119.4 no
C12 . C13 . N14 . 119.270(13) yes
C12 . C13 . H131 . 120.2 no
N14 . C13 . H131 . 120.5 no
Mn2 . N14 . C9 . 114.8(4) yes
Mn2 . N14 . C13 . 127.0(4) yes
C9 . N14 . C13 . 117.816(18) yes
Mn2 . N3 . C4 . 120.4(3) yes
Mn2 . N3 . C8 . 113.5(3) yes
C4 . N3 . C8 . 125.91(2) yes
N3 . C4 . C5 . 118.40(3) yes
N3 . C4 . H41 . 120.4 no
C5 . C4 . H41 . 121.2 no
C4 . C5 . C6 . 119.369(16) yes
C4 . C5 . H51 . 119.5 no
C6 . C5 . H51 . 121.1 no
C5 . C6 . C7 . 121.356(15) yes
C5 . C6 . H61 . 118.0 no
C7 . C6 . H61 . 120.6 no
C6 . C7 . C8 . 114.99(3) yes
C6 . C7 . H71 . 121.1 no
C8 . C7 . H71 . 123.9 no
C7 . C8 . C9 . 121.7(5) yes
C7 . C8 . N3 . 119.210(19) yes
C9 . C8 . N3 . 119.0(5) yes