# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full Chem.Commun.
_journal_coden_cambridge 0182
#TrackingRef '- crystal_structure.cif'
_publ_section_exptl_refinement
;
The SXRD analysis revealed that the crystal structure of trip-MOF-1 is built up
from two Co^II^ cations (Fig. 2a), one ttc anion, one metal-coordinated
water and N,N-dimethylformamide (DMF) solvent molecules. The Co^II^ centers
are located on special positions with a site-occupancy factor of 0.5. The Co1
atoms lie on two-fold axes while the Co2 atoms lie on centers of inversion.
Co1 is tetrahedrally coordinated by four carboxylate O atoms from four
different ttc ligands and Co2 is octahedrally coordinated by four
carboxylate O atoms from two different ttc ligands, one O atom from a
water molecule and one O atom from a DMF molecule. The trans water and
DMF ligands are disordered over two sets of sites with an occupancy of 0.5
while the ttc ligand is extensively disordered about a crystallographic
center of inversion. The Co cations are linked by the ttc anions into a
three-dimensional framework. In overall 3-D structural connectivity, Co1 and
Co2 centers essentially act as a tetrahedral and a square planar node (Fig.
2c), respectively.
A total number of 12 restraints (SADI, DFIX and DANG commands) had to be used
to correct the geometry of the disordered DMF, water and ttc ligands,
and the thermal parameters of the trans water and DMF molecules (see
_iucr_refine_instructions_details for the SHELXL97 input file at the end of
the CIF).
;
#Added by publCIF
_audit_update_record
;
2012-03-22 # Formatted by publCIF
;
#
#-------------------------------------------------------------------------
#2 Person making the deposition
#
_publ_contact_author 'Dr. Blacque, Olivier'
_publ_contact_author_email oblacque@aci.uzh.ch
_publ_contact_author_fax '+41 44 63 54 681'
_publ_contact_author_phone '+41 44 63 54 651'
#-------------------------------------------------------------------------
#3 Publication details
#
# Provide these details if the structure has been published,
# accepted or submitted for publication
#
# The CCDC journal deposition number, eg. 182/357,
# should be included only if it has been assigned by the journal
#
#
#-------------------------------------------------------------------------
#4 Chemical and physical data
#
# Note that the units for melting point are Kelvin
# The compound_id is the identifier for the compound in the published
# paper, eg. 4a, II, etc.
# Provide a brief description of any significant biological activity,
# eg. antimalarial activity
# If the compound exhibits polymorphism provide brief details,
# eg. monoclinic form, low-temperature phase, etc.
# For chemdiag leave blank - no longer necessary
#
#-------------------------------------------------------------------------
#5 Other data relating to the structure determination and refinement
#
# Record the radiation type if not X-rays, eg. neutron
# Record the temperature of the data collection (Kelvin)
# if not room-temperature
# Record R_squared if this is the only reliability factor given by
# your refinement program
# Describe briefly any disorder, eg. t-Butyl C31-33 disordered over
# two sites with occupancies 0.6 and 0.4
# Under ccdc_comments record any other important information
#-------------------------------------------------------------------------
#6 Include your "standard" CIF file here
# It should contain the following data items:
# unit cell parameters and volume, z value, space group symbol,
# R-factor(s), atomic coordinates with standard deviations,
# occupancy factors, bond lengths and bond angles
# Other data items may be present but will not necessarily be
# included in the Cambridge Structural Database
#
# Do NOT include structure factors
#
#
#-------------------------------------------------------------------------
#SUBMISSION INFORMATION
#
# For a journal send the form to the address specified by the journal
#
# For a private communication to the CCDC send the form to the address
# deposit@ccdc.cam.ac.uk
#
# For up-to-date information on deposition procedures, check the website
# http://www.ccdc.cam.ac.uk/
_publ_section_comment
;
(type here to add)
;
_publ_section_abstract
;
(type here to add abstract)
;
_publ_contact_letter
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;
# TITLE AND AUTHOR LIST
_publ_section_title
;
Triptycene based luminescent metal-organic gels for chemosensing
;
loop_
_publ_author_name
_publ_author_address
#Corresponding author of the paper
S.Barman
;
Institute of Inorganic Chemistry, Winterthurerstrasse 190,
CH-8057, Zuerich, Switzerland
;
J.A.Garg
;
Institute of Inorganic Chemistry, Winterthurerstrasse 190,
CH-8057, Zuerich, Switzerland
;
O.Blacque
;
Institute of Inorganic Chemistry, Winterthurerstrasse 190,
CH-8057, Zuerich, Switzerland
;
K.Venkatesan
;
Institute of Inorganic Chemistry, Winterthurerstrasse 190,
CH-8057, Zuerich, Switzerland
;
H.Berke
;
Institute of Inorganic Chemistry, Winterthurerstrasse 190,
CH-8057, Zuerich, Switzerland
;
_publ_contact_author_name 'Dr. Blacque, Olivier'
#------------------------------------------------------------#
data_1
_database_code_depnum_ccdc_archive 'CCDC 872964'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C27 H19 Co2 N O10'
_chemical_formula_sum 'C27 H19 Co2 N O10'
_chemical_formula_weight 635.29
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 17.1691(5)
_cell_length_b 11.0334(5)
_cell_length_c 16.3274(6)
_cell_angle_alpha 90.00
_cell_angle_beta 98.302(3)
_cell_angle_gamma 90.00
_cell_volume 3060.5(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 183(2)
_cell_measurement_reflns_used 3441
_cell_measurement_theta_min 2.44
_cell_measurement_theta_max 32.75
_exptl_crystal_description plate
_exptl_crystal_colour violet
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.379
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1288
_exptl_absorpt_coefficient_mu 1.135
_exptl_absorpt_correction_T_min 0.864
_exptl_absorpt_correction_T_max 0.975
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Version 1.171.33.66 (Agilent, 2011)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by Clark & Reid (1995).
;
_exptl_special_details ?
_diffrn_ambient_temperature 183(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method 'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9118
_diffrn_reflns_av_R_equivalents 0.0431
_diffrn_reflns_av_sigmaI/netI 0.0650
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.45
_diffrn_reflns_theta_max 25.00
_reflns_number_total 2691
_reflns_number_gt 1970
_reflns_threshold_expression >2sigma(I)
_computing_data_collection
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.33.55 (Agilent, 2011)
;
_computing_structure_solution
; SHELXS97. Sheldrick (2008)
;
_computing_structure_refinement
; SHELXL97. Sheldrick (2008).
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+11.3813P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2691
_refine_ls_number_parameters 254
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.1048
_refine_ls_R_factor_gt 0.0756
_refine_ls_wR_factor_ref 0.2256
_refine_ls_wR_factor_gt 0.2135
_refine_ls_goodness_of_fit_ref 1.107
_refine_ls_restrained_S_all 1.105
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0957(4) 0.3200(6) 0.1340(4) 0.0368(15) Uani 1 1 d . . .
C2 C 0.1693(4) 0.2485(7) 0.1290(4) 0.0391(16) Uani 1 1 d . . .
C5 C 0.3080(4) 0.1107(6) 0.1282(4) 0.0368(16) Uani 1 1 d . . .
C3A C 0.1842(9) 0.1489(17) 0.1777(11) 0.046(4) Uani 0.50 1 d P . .
H3A H 0.1483 0.1268 0.2126 0.056 Uiso 0.50 1 calc PR . .
C4A C 0.2528(11) 0.0776(18) 0.1770(12) 0.057(5) Uani 0.50 1 d P . .
H4A H 0.2604 0.0083 0.2096 0.069 Uiso 0.50 1 calc PR . .
C6A C 0.2968(6) 0.2161(12) 0.0806(8) 0.032(3) Uani 0.50 1 d P . .
C7A C 0.2285(7) 0.2884(11) 0.0816(7) 0.030(3) Uani 0.50 1 d P . .
C3B C 0.2138(9) 0.212(2) 0.2026(10) 0.053(5) Uani 0.50 1 d P . .
H3B H 0.1970 0.2317 0.2526 0.064 Uiso 0.50 1 calc PR . .
C4B C 0.2834(10) 0.1476(17) 0.2026(10) 0.050(4) Uani 0.50 1 d P . .
H4B H 0.3140 0.1286 0.2527 0.060 Uiso 0.50 1 calc PR . .
C6B C 0.2589(7) 0.1353(11) 0.0545(8) 0.031(3) Uani 0.50 1 d P . .
C7B C 0.1901(7) 0.2046(12) 0.0544(8) 0.030(3) Uani 0.50 1 d P . .
C8 C 0.3845(4) 0.0378(6) 0.1339(4) 0.0380(16) Uani 1 1 d . . .
C9 C 0.3553(7) 0.2764(11) 0.0296(7) 0.029(3) Uani 0.50 1 d P . .
H9 H 0.4034 0.2288 0.0288 0.035 Uiso 0.50 1 calc PR . .
C10 C 0.2275(7) 0.4018(12) 0.0320(8) 0.034(3) Uani 0.50 1 d P . .
H10 H 0.1795 0.4496 0.0324 0.041 Uiso 0.50 1 calc PR . .
C11 C 0.3034(4) 0.4723(7) 0.0659(6) 0.039(3) Uani 0.50 1 d PG . .
C12 C 0.3714(5) 0.4042(6) 0.0652(6) 0.032(3) Uani 0.50 1 d PG . .
C13 C 0.4446(4) 0.4555(8) 0.0919(6) 0.052(4) Uani 0.50 1 d PG . .
H13 H 0.4901 0.4099 0.0914 0.062 Uiso 0.50 1 calc PR . .
C14 C 0.4498(4) 0.5749(9) 0.1192(7) 0.074(6) Uani 0.50 1 d PG . .
H14 H 0.4988 0.6092 0.1370 0.089 Uiso 0.50 1 calc PR . .
C15 C 0.3818(6) 0.6430(6) 0.1199(7) 0.056(4) Uani 0.50 1 d PG . .
H15 H 0.3853 0.7229 0.1382 0.067 Uiso 0.50 1 calc PR . .
C16 C 0.3086(5) 0.5917(7) 0.0933(6) 0.047(4) Uani 0.50 1 d PG . .
H16 H 0.2631 0.6373 0.0937 0.056 Uiso 0.50 1 calc PR . .
O1 O 0.0609(3) 0.2966(5) 0.1939(3) 0.0534(14) Uani 1 1 d . . .
O2 O 0.0753(3) 0.3981(6) 0.0835(4) 0.080(2) Uani 1 1 d . A .
O3 O 0.4082(3) 0.0041(6) 0.0703(4) 0.078(2) Uani 1 1 d . . .
O4 O 0.4153(4) 0.0150(6) 0.2044(3) 0.080(2) Uani 1 1 d . . .
O5 O -0.0505(10) 0.3547(16) -0.0716(9) 0.079(5) Uani 0.50 1 d PD A -1
O6 O 0.054(2) 0.659(2) 0.0349(12) 0.138(5) Uani 0.50 1 d PD A -2
N1 N 0.1091(13) 0.7923(16) 0.1337(10) 0.138(5) Uani 0.50 1 d PD A -2
C17 C 0.0739(19) 0.699(2) 0.1021(12) 0.138(5) Uani 0.50 1 d PD A -2
H17 H 0.0600 0.6471 0.1427 0.165 Uiso 0.50 1 calc PR A -2
C18 C 0.1532(16) 0.852(2) 0.0922(14) 0.138(5) Uani 0.50 1 d PD A -2
H18A H 0.1671 0.8017 0.0483 0.206 Uiso 0.50 1 calc PR A -2
H18B H 0.2001 0.8758 0.1277 0.206 Uiso 0.50 1 calc PR A -2
H18C H 0.1258 0.9224 0.0690 0.206 Uiso 0.50 1 calc PR A -2
C19 C 0.1128(18) 0.812(2) 0.2108(13) 0.138(5) Uani 0.50 1 d PD A -2
H19A H 0.0968 0.8938 0.2195 0.206 Uiso 0.50 1 calc PR A -2
H19B H 0.1658 0.8001 0.2374 0.206 Uiso 0.50 1 calc PR A -2
H19C H 0.0785 0.7568 0.2337 0.206 Uiso 0.50 1 calc PR A -2
Co1 Co 0.0000 0.40958(12) 0.2500 0.0328(4) Uani 1 2 d S . .
Co2 Co 0.0000 0.5000 0.0000 0.0406(4) Uani 1 2 d SD . .
H5A H -0.085(6) 0.3928(17) -0.115(4) 0.061 Uiso 0.50 1 d PD B -1
H5B H -0.076(6) 0.309(6) -0.034(2) 0.061 Uiso 0.50 1 d PD C -1
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
C1 0.028(3) 0.049(4) 0.036(4) 0.000(3) 0.014(3) 0.004(3)
C2 0.030(3) 0.058(4) 0.033(4) 0.005(3) 0.017(3) 0.011(3)
C5 0.028(3) 0.048(4) 0.038(4) 0.009(3) 0.016(3) 0.012(3)
C3A 0.030(8) 0.062(11) 0.051(11) 0.028(9) 0.020(7) 0.005(8)
C4A 0.058(11) 0.055(12) 0.069(13) 0.039(10) 0.042(10) 0.030(9)
C6A 0.018(6) 0.046(8) 0.035(7) -0.004(6) 0.015(5) 0.002(6)
C7A 0.032(6) 0.032(7) 0.028(6) -0.004(5) 0.010(5) 0.003(6)
C3B 0.033(9) 0.102(16) 0.029(8) 0.005(9) 0.019(7) 0.019(10)
C4B 0.048(10) 0.059(12) 0.044(9) 0.017(9) 0.015(7) 0.027(9)
C6B 0.027(6) 0.030(7) 0.038(7) 0.003(6) 0.017(5) -0.001(6)
C7B 0.028(6) 0.034(7) 0.032(6) 0.006(6) 0.016(5) 0.006(6)
C8 0.028(3) 0.046(4) 0.043(4) 0.006(3) 0.016(3) 0.005(3)
C9 0.022(5) 0.036(7) 0.032(6) 0.002(5) 0.012(5) 0.000(5)
C10 0.027(6) 0.047(8) 0.032(7) -0.011(6) 0.015(5) -0.001(6)
C11 0.042(8) 0.043(8) 0.035(7) 0.003(6) 0.013(6) -0.002(6)
C12 0.038(7) 0.029(6) 0.031(6) -0.004(5) 0.012(5) -0.007(6)
C13 0.041(8) 0.063(10) 0.053(9) 0.005(8) 0.012(7) -0.003(8)
C14 0.063(11) 0.086(14) 0.071(12) -0.012(10) 0.003(9) -0.051(11)
C15 0.057(9) 0.052(9) 0.061(10) -0.031(8) 0.019(8) -0.018(8)
C16 0.071(10) 0.032(8) 0.038(8) -0.005(6) 0.013(7) 0.006(8)
O1 0.048(3) 0.065(3) 0.055(3) 0.014(3) 0.037(2) 0.020(3)
O2 0.061(3) 0.122(5) 0.068(4) 0.057(4) 0.043(3) 0.058(4)
O3 0.057(3) 0.127(6) 0.058(4) 0.032(4) 0.033(3) 0.056(4)
O4 0.071(4) 0.126(6) 0.040(3) -0.001(3) 0.000(3) 0.070(4)
O5 0.073(8) 0.075(11) 0.088(11) -0.044(10) 0.009(9) 0.022(8)
O6 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8)
N1 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8)
C17 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8)
C18 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8)
C19 0.202(13) 0.089(7) 0.115(10) 0.027(8) -0.003(10) -0.044(8)
Co1 0.0207(6) 0.0532(8) 0.0259(7) 0.000 0.0086(5) 0.000
Co2 0.0351(7) 0.0513(9) 0.0395(8) 0.0097(6) 0.0192(6) 0.0173(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.209(8) . ?
C1 O1 1.245(8) . ?
C1 C2 1.501(9) . ?
C2 C3A 1.360(17) . ?
C2 C3B 1.387(17) . ?
C2 C7B 1.404(14) . ?
C2 C7A 1.434(14) . ?
C5 C4A 1.372(17) . ?
C5 C6B 1.394(14) . ?
C5 C6A 1.398(15) . ?
C5 C4B 1.403(18) . ?
C5 C8 1.531(8) . ?
C3A C4A 1.42(2) . ?
C3A H3A 0.9300 . ?
C4A H4A 0.9300 . ?
C6A C6B 1.150(17) . ?
C6A C7A 1.420(16) . ?
C6A C9 1.544(16) . ?
C6A C7B 1.826(16) . ?
C7A C7B 1.185(17) . ?
C7A C10 1.489(18) . ?
C7A C6B 1.841(17) . ?
C3B C4B 1.39(2) . ?
C3B H3B 0.9300 . ?
C4B H4B 0.9300 . ?
C6B C7B 1.407(16) . ?
C6B C10 1.520(17) 7 ?
C7B C9 1.491(17) 7 ?
C8 O4 1.222(9) . ?
C8 O3 1.227(9) . ?
C9 C7B 1.491(17) 7 ?
C9 C12 1.534(14) . ?
C9 H9 0.9800 . ?
C10 C6B 1.520(17) 7 ?
C10 C11 1.549(13) . ?
C10 H10 0.9800 . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 C15 1.3900 . ?
C14 H14 0.9300 . ?
C15 C16 1.3900 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
O1 Co1 1.939(5) . ?
O2 Co2 2.070(5) . ?
O3 Co2 2.079(5) 3_545 ?
O4 Co1 1.925(5) 3_545 ?
O5 Co2 2.096(16) . ?
O5 H5A 0.950(5) . ?
O5 H5B 0.949(5) . ?
O6 C17 1.186(10) . ?
O6 Co2 2.02(2) . ?
N1 C18 1.269(16) . ?
N1 C17 1.269(16) . ?
N1 C19 1.270(16) . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
Co1 O4 1.925(5) 4 ?
Co1 O4 1.925(5) 3_455 ?
Co1 O1 1.939(5) 2 ?
Co2 O6 2.02(2) 5_565 ?
Co2 O2 2.070(5) 5_565 ?
Co2 O3 2.079(5) 3_455 ?
Co2 O3 2.079(5) 7 ?
Co2 O5 2.096(16) 5_565 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 124.0(6) . . ?
O2 C1 C2 120.0(6) . . ?
O1 C1 C2 116.0(6) . . ?
C3A C2 C7B 100.3(10) . . ?
C3B C2 C7B 118.3(9) . . ?
C3A C2 C7A 118.4(9) . . ?
C3B C2 C7A 102.1(9) . . ?
C3A C2 C1 118.8(8) . . ?
C3B C2 C1 117.8(8) . . ?
C7B C2 C1 123.4(7) . . ?
C7A C2 C1 122.5(7) . . ?
C4A C5 C6B 99.8(10) . . ?
C4A C5 C6A 119.6(9) . . ?
C6B C5 C4B 118.1(9) . . ?
C6A C5 C4B 101.8(10) . . ?
C4A C5 C8 118.9(8) . . ?
C6B C5 C8 124.1(7) . . ?
C6A C5 C8 121.2(7) . . ?
C4B C5 C8 117.7(8) . . ?
C2 C3A C4A 122.0(13) . . ?
C2 C3A H3A 119.0 . . ?
C4A C3A H3A 119.0 . . ?
C5 C4A C3A 120.1(13) . . ?
C5 C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C6B C6A C5 65.5(10) . . ?
C6B C6A C7A 90.9(10) . . ?
C5 C6A C7A 120.6(10) . . ?
C6B C6A C9 120.8(12) . . ?
C5 C6A C9 127.6(9) . . ?
C7A C6A C9 111.5(11) . . ?
C5 C6A C7B 97.2(8) . . ?
C9 C6A C7B 127.8(10) . . ?
C7B C7A C6A 88.5(10) . . ?
C6A C7A C2 119.0(10) . . ?
C7B C7A C10 119.3(12) . . ?
C6A C7A C10 114.2(11) . . ?
C2 C7A C10 126.7(10) . . ?
C2 C7A C6B 95.5(8) . . ?
C10 C7A C6B 128.5(9) . . ?
C2 C3B C4B 121.0(13) . . ?
C2 C3B H3B 119.5 . . ?
C4B C3B H3B 119.5 . . ?
C3B C4B C5 121.0(14) . . ?
C3B C4B H4B 119.5 . . ?
C5 C4B H4B 119.5 . . ?
C6A C6B C5 65.8(9) . . ?
C6A C6B C7B 90.5(11) . . ?
C5 C6B C7B 120.7(11) . . ?
C6A C6B C10 113.5(12) . 7 ?
C5 C6B C10 126.5(10) . 7 ?
C7B C6B C10 112.7(11) . 7 ?
C5 C6B C7A 97.3(9) . . ?
C10 C6B C7A 123.8(10) 7 . ?
C7A C7B C6B 90.1(11) . . ?
C2 C7B C6B 120.3(10) . . ?
C7A C7B C9 115.1(11) . 7 ?
C2 C7B C9 125.8(9) . 7 ?
C6B C7B C9 113.9(11) . 7 ?
C2 C7B C6A 98.3(9) . . ?
C9 C7B C6A 125.4(9) 7 . ?
O4 C8 O3 125.7(6) . . ?
O4 C8 C5 114.6(6) . . ?
O3 C8 C5 119.7(6) . . ?
C7B C9 C12 105.1(10) 7 . ?
C7B C9 C6A 105.2(9) 7 . ?
C12 C9 C6A 106.7(9) . . ?
C7B C9 H9 113.1 7 . ?
C12 C9 H9 113.1 . . ?
C6A C9 H9 113.1 . . ?
C7A C10 C6B 106.7(10) . 7 ?
C7A C10 C11 106.5(10) . . ?
C6B C10 C11 103.5(9) 7 . ?
C7A C10 H10 113.1 . . ?
C6B C10 H10 113.1 7 . ?
C11 C10 H10 113.1 . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C10 112.9(7) . . ?
C16 C11 C10 127.0(7) . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C9 113.2(7) . . ?
C13 C12 C9 126.7(7) . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.0 . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C1 O1 Co1 126.2(5) . . ?
C1 O2 Co2 158.1(6) . . ?
C8 O3 Co2 147.6(6) . 3_545 ?
C8 O4 Co1 133.6(5) . 3_545 ?
Co2 O5 H5A 103.8(12) . . ?
Co2 O5 H5B 103.9(12) . . ?
H5A O5 H5B 114.7(14) . . ?
C17 O6 Co2 130(2) . . ?
C18 N1 C17 119.3(7) . . ?
C18 N1 C19 119.6(7) . . ?
C17 N1 C19 119.7(7) . . ?
O6 C17 N1 137(2) . . ?
O6 C17 H17 111.3 . . ?
N1 C17 H17 111.3 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 Co1 O4 105.7(4) 4 3_455 ?
O4 Co1 O1 98.2(3) 4 . ?
O4 Co1 O1 129.3(2) 3_455 . ?
O4 Co1 O1 129.3(2) 4 2 ?
O4 Co1 O1 98.2(3) 3_455 2 ?
O1 Co1 O1 100.0(3) . 2 ?
O6 Co2 O6 180.000(2) . 5_565 ?
O6 Co2 O2 93.8(8) . . ?
O6 Co2 O2 86.2(8) 5_565 . ?
O6 Co2 O2 86.2(8) . 5_565 ?
O6 Co2 O2 93.8(8) 5_565 5_565 ?
O2 Co2 O2 180.0 . 5_565 ?
O6 Co2 O3 100.3(9) . 3_455 ?
O6 Co2 O3 79.7(9) 5_565 3_455 ?
O2 Co2 O3 95.7(2) . 3_455 ?
O2 Co2 O3 84.3(2) 5_565 3_455 ?
O6 Co2 O3 79.7(9) . 7 ?
O6 Co2 O3 100.3(9) 5_565 7 ?
O2 Co2 O3 84.3(2) . 7 ?
O2 Co2 O3 95.7(2) 5_565 7 ?
O3 Co2 O3 180.0(5) 3_455 7 ?
O6 Co2 O5 17.4(8) . 5_565 ?
O6 Co2 O5 162.6(8) 5_565 5_565 ?
O2 Co2 O5 83.1(5) . 5_565 ?
O2 Co2 O5 96.9(5) 5_565 5_565 ?
O3 Co2 O5 87.8(5) 3_455 5_565 ?
O3 Co2 O5 92.2(5) 7 5_565 ?
O6 Co2 O5 162.6(8) . . ?
O6 Co2 O5 17.4(8) 5_565 . ?
O2 Co2 O5 96.9(5) . . ?
O2 Co2 O5 83.1(5) 5_565 . ?
O3 Co2 O5 92.2(5) 3_455 . ?
O3 Co2 O5 87.8(5) 7 . ?
O5 Co2 O5 180.000(1) 5_565 . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.796
_refine_diff_density_min -0.728
_refine_diff_density_rms 0.129
########################################################################
_publ_section_references
;
Agilent (2011). CrysAlis PRO. Agilent Technologies, Yarnton, England.
Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887--897.
Farrugia, L. J. (1997). J. Appl. Cryst. 32, 565--?.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7--13.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920--925.
;
########################################################################
_iucr_refine_instructions_details
;
TITL sami1602 in C2/c
CELL 0.71073 17.1691 11.0334 16.3274 90.000 98.302 90.000
ZERR 4.00 0.0005 0.0005 0.0006 0.000 0.003 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H CO N O
UNIT 108 76 8 4 40
MERG 2
OMIT -2.00 50.00
OMIT 0 0 4
OMIT -2 0 2
SADI 0.005 N1 C17 N1 C18 N1 C19
SADI 0.010 C17 C18 C18 C19 C17 C19
EADP O6 C17 N1 C18 C19
DFIX 1.20 0.010 C17 O6
FREE C3A C3B C3A C4B
FREE C4A C4B C4A C3B
DFIX 0.95 0.005 O5 H5A O5 H5B
DANG 2.50 0.005 CO2 H5A CO2 H5B
DANG 1.60 0.010 H5A H5B
FMAP 2
PLAN 20
ACTA
BOND $H
L.S. 8
WGHT 0.121900 11.381301
FVAR 0.49133
C1 1 0.095679 0.319963 0.133999 11.00000 0.02815 0.04872 =
0.03635 0.00021 0.01442 0.00362
C2 1 0.169266 0.248518 0.128957 11.00000 0.02963 0.05801 =
0.03318 0.00521 0.01666 0.01134
C5 1 0.308022 0.110663 0.128240 11.00000 0.02789 0.04768 =
0.03804 0.00852 0.01583 0.01172
C3A 1 0.184201 0.148895 0.177706 10.50000 0.02957 0.06224 =
0.05130 0.02818 0.02030 0.00484
AFIX 43
H3A 2 0.148311 0.126837 0.212600 10.50000 -1.20000
AFIX 0
C4A 1 0.252838 0.077559 0.176987 10.50000 0.05809 0.05478 =
0.06867 0.03897 0.04183 0.03046
AFIX 43
H4A 2 0.260439 0.008271 0.209597 10.50000 -1.20000
AFIX 0
C6A 1 0.296826 0.216143 0.080587 10.50000 0.01813 0.04614 =
0.03490 -0.00383 0.01485 0.00176
C7A 1 0.228546 0.288420 0.081561 10.50000 0.03158 0.03208 =
0.02842 -0.00443 0.00970 0.00346
C3B 1 0.213847 0.212355 0.202551 10.50000 0.03309 0.10174 =
0.02925 0.00474 0.01900 0.01911
AFIX 43
H3B 2 0.197012 0.231653 0.252602 10.50000 -1.20000
AFIX 0
C4B 1 0.283373 0.147642 0.202585 10.50000 0.04826 0.05934 =
0.04370 0.01686 0.01511 0.02668
AFIX 43
H4B 2 0.313985 0.128600 0.252667 10.50000 -1.20000
AFIX 0
C6B 1 0.258873 0.135252 0.054464 10.50000 0.02717 0.03027 =
0.03819 0.00266 0.01749 -0.00051
C7B 1 0.190065 0.204591 0.054361 10.50000 0.02821 0.03388 =
0.03204 0.00569 0.01646 0.00645
C8 1 0.384524 0.037847 0.133866 11.00000 0.02782 0.04598 =
0.04342 0.00560 0.01635 0.00504
C9 1 0.355343 0.276400 0.029648 10.50000 0.02193 0.03636 =
0.03228 0.00150 0.01151 0.00022
AFIX 13
H9 2 0.403413 0.228808 0.028795 10.50000 -1.20000
AFIX 0
C10 1 0.227547 0.401816 0.031990 10.50000 0.02705 0.04681 =
0.03177 -0.01097 0.01541 -0.00110
AFIX 13
H10 2 0.179500 0.449640 0.032356 10.50000 -1.20000
AFIX 66
C11 1 0.303417 0.472264 0.065924 10.50000 0.04205 0.04281 =
0.03498 0.00265 0.01337 -0.00159
C12 1 0.371427 0.404161 0.065218 10.50000 0.03790 0.02860 =
0.03103 -0.00365 0.01219 -0.00700
C13 1 0.444642 0.455484 0.091858 10.50000 0.04081 0.06250 =
0.05339 0.00533 0.01210 -0.00327
AFIX 43
H13 2 0.490145 0.409918 0.091385 10.50000 -1.20000
AFIX 65
C14 1 0.449847 0.574909 0.119205 10.50000 0.06278 0.08576 =
0.07128 -0.01197 0.00315 -0.05083
AFIX 43
H14 2 0.498833 0.609247 0.137029 10.50000 -1.20000
AFIX 65
C15 1 0.381838 0.643013 0.119912 10.50000 0.05654 0.05223 =
0.06128 -0.03066 0.01893 -0.01774
AFIX 43
H15 2 0.385321 0.722917 0.138209 10.50000 -1.20000
AFIX 65
C16 1 0.308623 0.591692 0.093271 10.50000 0.07115 0.03239 =
0.03782 -0.00518 0.01286 0.00575
AFIX 43
H16 2 0.263120 0.637259 0.093744 10.50000 -1.20000
AFIX 0
O1 5 0.060857 0.296646 0.193935 11.00000 0.04819 0.06536 =
0.05545 0.01432 0.03722 0.02041
O2 5 0.075315 0.398119 0.083499 11.00000 0.06065 0.12156 =
0.06779 0.05733 0.04290 0.05777
O3 5 0.408215 0.004127 0.070251 11.00000 0.05698 0.12722 =
0.05835 0.03213 0.03273 0.05642
O4 5 0.415338 0.014955 0.204372 11.00000 0.07071 0.12641 =
0.04025 -0.00076 0.00030 0.07049
PART -1
O5 5 -0.050468 0.354744 -0.071596 10.50000 0.07326 0.07510 =
0.08821 -0.04393 0.00893 0.02245
PART -2
O6 5 0.053977 0.658536 0.034913 10.50000 0.20157 0.08858 =
0.11470 0.02705 -0.00317 -0.04368
N1 4 0.109112 0.792288 0.133687 10.50000 0.20157 0.08858 =
0.11470 0.02705 -0.00317 -0.04368
C17 1 0.073932 0.698535 0.102065 10.50000 0.20157 0.08858 =
0.11470 0.02705 -0.00317 -0.04368
AFIX 43
H17 2 0.059992 0.647144 0.142702 10.50000 -1.20000
AFIX 0
C18 1 0.153216 0.851678 0.092153 10.50000 0.20157 0.08858 =
0.11470 0.02705 -0.00317 -0.04368
AFIX 137
H18A 2 0.167088 0.801742 0.048324 10.50000 -1.50000
H18B 2 0.200123 0.875831 0.127709 10.50000 -1.50000
H18C 2 0.125796 0.922383 0.069011 10.50000 -1.50000
AFIX 0
C19 1 0.112778 0.811949 0.210759 10.50000 0.20157 0.08858 =
0.11470 0.02705 -0.00317 -0.04368
AFIX 137
H19A 2 0.096801 0.893762 0.219479 10.50000 -1.50000
H19B 2 0.165849 0.800143 0.237366 10.50000 -1.50000
H19C 2 0.078457 0.756810 0.233715 10.50000 -1.50000
AFIX 0
PART 0
CO1 3 0.000000 0.409583 0.250000 10.50000 0.02072 0.05317 =
0.02595 0.00000 0.00855 0.00000
CO2 3 0.000000 0.500000 0.000000 10.50000 0.03510 0.05128 =
0.03951 0.00974 0.01920 0.01728
PART -1
H5A 2 -0.085163 0.392797 -0.114569 10.50000 -1.50000
H5B 2 -0.075789 0.308612 -0.034033 10.50000 -1.50000
HKLF 4
REM sami1602 in C2/c
REM R1 = 0.0756 for 1970 Fo > 4sig(Fo) and 0.1048 for all 2691 data
REM 254 parameters refined using 12 restraints
END
WGHT 0.1200 13.3751
REM Highest difference peak 0.796, deepest hole -0.728, 1-sigma level 0.129
Q1 1 0.0000 0.4991 0.2500 10.50000 0.05 0.80
Q2 1 0.0984 0.7022 0.0757 11.00000 0.05 0.72
Q3 1 0.3310 0.5538 0.0802 11.00000 0.05 0.71
Q4 1 0.2506 0.5691 0.0679 11.00000 0.05 0.70
Q5 1 -0.0026 0.5923 0.0071 11.00000 0.05 0.58
Q6 1 0.2295 0.6593 0.0806 11.00000 0.05 0.55
Q7 1 0.3985 0.6095 0.0998 11.00000 0.05 0.53
Q8 1 0.4325 0.0769 0.0928 11.00000 0.05 0.53
Q9 1 0.0425 0.7650 0.2045 11.00000 0.05 0.52
Q10 1 -0.0164 0.3398 -0.0667 11.00000 0.05 0.47
Q11 1 0.0568 0.8507 0.1024 11.00000 0.05 0.47
Q12 1 0.1812 0.8690 0.1483 11.00000 0.05 0.41
Q13 1 -0.0607 0.4165 -0.0793 11.00000 0.05 0.41
Q14 1 0.0314 0.7666 0.0708 11.00000 0.05 0.41
Q15 1 0.4289 0.4050 0.0824 11.00000 0.05 0.40
Q16 1 0.4408 0.5679 0.1387 11.00000 0.05 0.39
Q17 1 0.3773 0.4612 0.0529 11.00000 0.05 0.38
Q18 1 0.0469 0.3199 0.0773 11.00000 0.05 0.36
Q19 1 0.0883 0.9198 0.2817 11.00000 0.05 0.33
Q20 1 0.1584 0.7764 0.0671 11.00000 0.05 0.31
;