# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full Chem.Commun.
_journal_coden_cambridge 0182
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_contact_author_address
;
Dr Stephen Moggach
RSE Personal Research Fellow
The University of Edinburgh
Joseph Black Building
West Mains Road
Edinburgh
EH9 3JJ
;
_publ_contact_author_email smoggach@staffmail.ed.ac.uk
_publ_contact_author_phone '+44(0)131 6504806'
#looking for refcif
_publ_contact_author_name 'Stephen A. Moggach'
loop_
_publ_author_name
'Thomas Bennett'
'Petra Simoncic'
'Stephen Moggach'
'Fabia Gozzo'
'Piero Macchi'
'David Keen'
J.C.Tan
'Tony Cheetham'
data_phaseIII_439
_database_code_depnum_ccdc_archive 'CCDC 828168'
#TrackingRef '- phaseIII_439.cif'
_audit_creation_date 11-03-21
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title 'phase3 in P2(1)/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.00
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6].. 14.96 Deg.
026_ALERT_3_A Ratio Observed / Unique Reflections too Low .... 0 Perc.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 11.22 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.61
088_ALERT_3_A Poor Data / Parameter Ratio .................... 2.74
201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 40
341_ALERT_3_A Low Bond Precision on C-C Bonds (x 1000) Ang ... 94
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.375 785
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 230
909_ALERT_3_G Percentage of Observed Data at Theta(Max) ...... 36.24
All of the above are caused by shading from the pressure cell. 1,2 and 1,3
restraints were applied to all non-hydrogen distances.
411_ALERT_2_A Short Inter H...H Contact H51 .. H201 .. 1.77 Ang.
413_ALERT_2_A Short Inter XH3 .. XHn H2023 .. H151 .. 1.77 Ang.
432_ALERT_2_A Short Inter X...Y Contact C5 .. C103 .. 2.86 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2011 .. H41 .. 2.06 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2011 .. H71 .. 2.02 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2012 .. H41 .. 2.08 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H1011 .. H131 .. 1.98 Ang.
432_ALERT_2_B Short Inter X...Y Contact O2 .. C3 .. 2.90 Ang.
432_ALERT_2_B Short Inter X...Y Contact C20 .. C103 .. 3.07 Ang.
410_ALERT_2_C Short Intra H...H Contact H11 .. H171 .. 1.94 Ang.
411_ALERT_2_C Short Inter H...H Contact H1031 .. H51 .. 2.05 Ang.
413_ALERT_2_C Short Inter XH3 .. XHn H2013 .. H71 .. 2.12 Ang.
432_ALERT_2_C Short Inter X...Y Contact O2 .. C20 .. 2.95 Ang.
432_ALERT_2_C Short Inter X...Y Contact N15 .. C104 .. 3.04 Ang.
432_ALERT_2_C Short Inter X...Y Contact C4 .. C201 .. 3.17 Ang.
432_ALERT_2_C Short Inter X...Y Contact C7 .. C201 .. 3.10 Ang.
Short contacts are expected at high-pressure.
082_ALERT_2_C High R1 Value .................................. 0.15
084_ALERT_2_C High R2 Value .................................. 0.33
The sample has undergone tow phase transitions which caused the crystal to
'break up', increasing the R1 value and increasing e.s.d's on measured
unit cell dimensions.
241_ALERT_2_C Check High Ueq as Compared to Neighbors for Zn4
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zn2
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2
No action taken.
731_ALERT_1_A Bond Calc 1.36(8), Rep 1.346(8) ...... 9.90 su-Ra
C1 -N2 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.356(8) ...... 8.75 su-Ra
C2 -C3 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(8), Rep 1.355(8) ...... 9.90 su-Ra
C2 -N1 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.341(8) ...... 9.90 su-Ra
C4 -N3 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(12), Rep 1.344(8) ...... 9.90 su-Ra
C4 -N4 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(11), Rep 1.355(8) ...... 9.90 su-Ra
C5 -C6 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.354(8) ...... 9.90 su-Ra
C5 -N3 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.352(8) ...... 9.90 su-Ra
C6 -N4 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(11), Rep 1.345(8) ...... 9.90 su-Ra
C7 -N5 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.346(8) ...... 9.90 su-Ra
C7 -N6 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(10), Rep 1.357(8) ...... 9.90 su-Ra
C8 -C9 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(10), Rep 1.352(8) ...... 9.90 su-Ra
C8 -N6 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(9), Rep 1.353(8) ...... 9.90 su-Ra
C9 -N5 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.344(8) ...... 9.90 su-Ra
C10 -N7 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.345(8) ...... 9.90 su-Ra
C10 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.355(8) ...... 9.90 su-Ra
C11 -C12 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(13), Rep 1.352(8) ...... 9.90 su-Ra
C11 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(9), Rep 1.353(8) ...... 9.90 su-Ra
C12 -N7 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.345(8) ...... 9.90 su-Ra
C13 -N9 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(8), Rep 1.344(8) ...... 9.90 su-Ra
C13 -N10 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(9), Rep 1.357(8) ...... 9.90 su-Ra
C14 -C15 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(11), Rep 1.352(8) ...... 9.90 su-Ra
C14 -N10 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(9), Rep 1.351(8) ...... 9.90 su-Ra
C15 -N9 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.345(8) ...... 9.90 su-Ra
C16 -N11 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.346(8) ...... 9.90 su-Ra
C16 -N12 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.356(8) ...... 8.75 su-Ra
C17 -C18 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(10), Rep 1.351(8) ...... 9.90 su-Ra
C17 -N12 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(8), Rep 1.351(8) ...... 9.90 su-Ra
C18 -N11 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.343(8) ...... 9.90 su-Ra
C19 -N13 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(10), Rep 1.344(8) ...... 9.90 su-Ra
C19 -N14 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.357(8) ...... 9.90 su-Ra
C20 -C21 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(10), Rep 1.353(8) ...... 9.90 su-Ra
C20 -N13 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.352(8) ...... 9.90 su-Ra
C21 -N14 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.344(8) ...... 9.90 su-Ra
C22 -N15 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.345(8) ...... 9.90 su-Ra
C22 -N16 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(10), Rep 1.356(8) ...... 9.90 su-Ra
C23 -C24 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(11), Rep 1.351(8) ...... 9.90 su-Ra
C23 -N15 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(10), Rep 1.351(8) ...... 9.90 su-Ra
C24 -N16 1.555 1.555
731_ALERT_1_A Bond Calc 1.50(15), Rep 1.498(8) ...... 9.90 su-Ra
C101 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(14), Rep 1.471(8) ...... 9.90 su-Ra
C102 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(11), Rep 1.460(8) ...... 9.90 su-Ra
C103 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(14), Rep 1.160(8) ...... 9.90 su-Ra
C103 -O2 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(10), Rep 1.459(8) ...... 9.90 su-Ra
C104 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(13), Rep 1.162(8) ...... 9.90 su-Ra
C104 -O1 1.555 1.555
731_ALERT_1_A Bond Calc 1.51(11), Rep 1.498(8) ...... 9.90 su-Ra
C201 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(13), Rep 1.468(8) ...... 9.90 su-Ra
C202 -N18 1.555 1.555
732_ALERT_1_A Angle Calc 113(7), Rep 112.7(6) ...... 9.90 su-Ra
N3 -C4 -N4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C6 -C5 -N3 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C5 -C6 -N4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 113(6), Rep 112.7(6) ...... 9.90 su-Ra
N5 -C7 -N6 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(5), Rep 109.1(6) ...... 8.33 su-Ra
C9 -C8 -N6 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C8 -C9 -N5 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 113(6), Rep 112.9(7) ...... 8.57 su-Ra
N7 -C10 -N8 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C12 -C11 -N8 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.3(6) ...... 9.90 su-Ra
C11 -C12 -N7 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 113(6), Rep 112.8(6) ...... 9.90 su-Ra
N9 -C13 -N10 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(5), Rep 109.1(6) ...... 8.33 su-Ra
C15 -C14 -N10 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C14 -C15 -N9 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 112(5), Rep 112.7(6) ...... 8.33 su-Ra
N11 -C16 -N12 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(5), Rep 109.1(6) ...... 8.33 su-Ra
C18 -C17 -N12 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(5), Rep 109.1(6) ...... 8.33 su-Ra
C17 -C18 -N11 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 113(5), Rep 113.2(6) ...... 8.33 su-Ra
N13 -C19 -N14 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(6), Rep 109.2(6) ...... 9.90 su-Ra
C21 -C20 -N13 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(6), Rep 109.1(6) ...... 9.90 su-Ra
C20 -C21 -N14 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 112(5), Rep 112.6(6) ...... 8.33 su-Ra
N15 -C22 -N16 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C24 -C23 -N15 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 109(6), Rep 109.0(6) ...... 9.90 su-Ra
C23 -C24 -N16 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 119(9), Rep 118.0(8) ...... 9.90 su-Ra
N17 -C103 -O2 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.3(5) ...... 9.90 su-Ra
C2 -N1 -C1 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(6), Rep 104.6(6) ...... 9.90 su-Ra
C5 -N3 -C4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(6), Rep 104.7(6) ...... 9.90 su-Ra
C6 -N4 -C4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(6), Rep 104.6(6) ...... 9.90 su-Ra
C9 -N5 -C7 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(6), Rep 104.6(6) ...... 9.90 su-Ra
C8 -N6 -C7 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 104(6), Rep 104.3(6) ...... 9.90 su-Ra
C12 -N7 -C10 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.6(6) ...... 8.33 su-Ra
C15 -N9 -C13 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 104(6), Rep 104.4(6) ...... 9.90 su-Ra
C14 -N10 -C13 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.6(6) ...... 8.33 su-Ra
C17 -N12 -C16 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 104(5), Rep 104.2(5) ...... 9.90 su-Ra
C20 -N13 -C19 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 104(5), Rep 104.3(6) ...... 8.33 su-Ra
C21 -N14 -C19 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.7(5) ...... 9.90 su-Ra
C23 -N15 -C22 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.7(6) ...... 8.33 su-Ra
C24 -N16 -C22 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 124(8), Rep 124.1(8) ...... 9.90 su-Ra
C101 -N17 -C102 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(8), Rep 109.9(8) ...... 9.90 su-Ra
C101 -N17 -C103 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 122(8), Rep 122.1(8) ...... 9.90 su-Ra
C102 -N17 -C103 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 124(8), Rep 123.7(8) ...... 9.90 su-Ra
C201 -N18 -C202 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(7), Rep 110.1(8) ...... 8.75 su-Ra
C201 -N18 -C104 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 122(7), Rep 122.0(8) ...... 8.75 su-Ra
C202 -N18 -C104 1.555 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.346(8) ...... 7.50 su-Ra
C1 -N1 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.350(8) ...... 7.50 su-Ra
C3 -N2 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.8(6) ...... 6.67 su-Ra
N1 -C1 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.2(6) ...... 5.00 su-Ra
C3 -C2 -N1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(4), Rep 109.1(6) ...... 6.67 su-Ra
C2 -C3 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.6(5) ...... 8.00 su-Ra
C3 -N2 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(6), Rep 104.5(8) ...... 7.50 su-Ra
C11 -N8 -C10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(6) ...... 6.67 su-Ra
C18 -N11 -C16 1.555 1.555 1.555
722_ALERT_1_C Angle Calc 125.00, Rep 123.80 Dev... 1.20 Deg.
N11 -C16 -H161 1.555 1.555 1.555
722_ALERT_1_C Angle Calc 124.00, Rep 125.30 Dev... 1.30 Deg.
C18 -C17 -H171 1.555 1.555 1.555
722_ALERT_1_C Angle Calc 124.00, Rep 125.40 Dev... 1.40 Deg.
N13 -C20 -H201 1.555 1.555 1.555
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 is badly in error.
153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 800 Ang.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C201
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C202
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C101
092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.69 Ang.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
These are correct.
720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 14
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 17.563(8)
_cell_length_b 13.825(8)
_cell_length_c 13.882(8)
_cell_angle_alpha 90
_cell_angle_beta 102.36(5)
_cell_angle_gamma 90
_cell_volume 3293(3)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 1 21/c 1 '
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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 0.0029 0.0015 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 0.0057 0.0031 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 0.0101 0.0057 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'
Zn 0.3006 1.3591 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C38 H40 N10 O2 Zn4
# Dc = 1.88 Fooo = 1920.00 Mu = 29.35 M = 930.32
# Found Formula = C30 H38 N18 O2 Zn4
# Dc = 1.90 FOOO = 1920.00 Mu = 29.43 M = 944.27
_chemical_formula_sum 'C30 H38 N18 O2 Zn4'
_chemical_formula_moiety 'C30 H38 N18 O2 Zn4'
_chemical_compound_source ?
_chemical_formula_weight 944.27
_cell_measurement_reflns_used 612
_cell_measurement_theta_min 3
_cell_measurement_theta_max 15
_cell_measurement_temperature 293
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 1.905
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.943
# Sheldrick geometric approximatio 0.56 0.75
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.41
_exptl_absorpt_correction_T_max 0.75
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.68890
_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 'USER DEFINED 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 293
_diffrn_reflns_number 740
_reflns_number_total 0
_diffrn_reflns_av_R_equivalents 0.000
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 736
# Theoretical number of reflections is about 1451
_diffrn_reflns_theta_min 1.834
_diffrn_reflns_theta_max 14.958
_diffrn_measured_fraction_theta_max 0.509
_diffrn_reflns_theta_full 11.218
_diffrn_measured_fraction_theta_full 0.613
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 10
_reflns_limit_h_min -12
_reflns_limit_h_max 12
_reflns_limit_k_min 0
_reflns_limit_k_max 9
_reflns_limit_l_min 0
_reflns_limit_l_max 10
_oxford_diffrn_Wilson_B_factor 6.04
_oxford_diffrn_Wilson_scale 153.08
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.60
_refine_diff_density_max 0.74
# 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>-10.0\s(I)
_refine_ls_number_reflns 651
_refine_ls_number_restraints 230
_refine_ls_number_parameters 238
_oxford_refine_ls_R_factor_ref 0.1922
_refine_ls_wR_factor_ref 0.3254
_refine_ls_goodness_of_fit_ref 1.0606
_refine_ls_shift/su_max 0.0245593
_refine_ls_shift/su_mean 0.0017714
# The values computed from all data
_oxford_reflns_number_all 651
_refine_ls_R_factor_all 0.1922
_refine_ls_wR_factor_all 0.3254
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 437
_refine_ls_R_factor_gt 0.1513
_refine_ls_wR_factor_gt 0.2994
# 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 Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
16.8 17.6 6.43
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.2043(9) 1.0289(9) 0.3984(10) 0.1107 1.0000 Uani . . . . . . .
Zn2 Zn 0.0601(8) 0.7218(9) 0.5873(10) 0.1105 1.0000 Uani . . . . . . .
Zn3 Zn 0.2915(8) 0.9545(9) 0.8588(10) 0.1087 1.0000 Uani . . . . . . .
Zn4 Zn 0.4189(9) 1.1919(10) 0.2088(11) 0.1258 1.0000 Uani . . . . . . .
C1 C 0.328(3) 1.121(3) 0.327(3) 0.070(13) 1.0000 Uiso D U . . . . .
C2 C 0.389(4) 1.015(2) 0.426(2) 0.070(13) 1.0000 Uiso D U . . . . .
C3 C 0.441(2) 1.062(3) 0.383(3) 0.070(13) 1.0000 Uiso D U . . . . .
C4 C 0.116(4) 0.866(6) 0.4776(16) 0.14(2) 1.0000 Uiso D U . . . . .
C5 C 0.231(3) 0.825(7) 0.4675(15) 0.14(2) 1.0000 Uiso D U . . . . .
C6 C 0.193(5) 0.745(4) 0.4885(15) 0.14(2) 1.0000 Uiso D U . . . . .
C7 C 0.075(4) 1.166(5) 0.4267(18) 0.107(16) 1.0000 Uiso D U . . . . .
C8 C 0.126(5) 1.296(3) 0.4923(19) 0.107(16) 1.0000 Uiso D U . . . . .
C9 C 0.184(3) 1.234(6) 0.483(2) 0.107(16) 1.0000 Uiso D U . . . . .
C10 C 0.133(3) 0.916(3) 0.212(7) 0.110(16) 1.0000 Uiso D U . . . . .
C11 C 0.063(2) 1.021(7) 0.122(5) 0.110(16) 1.0000 Uiso D U . . . . .
C12 C 0.102(4) 1.065(3) 0.205(6) 0.110(16) 1.0000 Uiso D U . . . . .
C13 C 0.179(4) 0.845(4) 0.730(4) 0.140(19) 1.0000 Uiso D U . . . . .
C14 C 0.114(5) 0.905(4) 0.829(3) 0.140(19) 1.0000 Uiso D U . . . . .
C15 C 0.068(3) 0.841(5) 0.769(5) 0.140(19) 1.0000 Uiso D U . . . . .
C16 C 0.359(3) 1.085(3) 0.032(5) 0.104(15) 1.0000 Uiso D U . . . . .
C17 C 0.268(4) 1.100(3) 0.111(3) 0.104(15) 1.0000 Uiso D U . . . . .
C18 C 0.243(3) 1.039(3) 0.034(4) 0.104(15) 1.0000 Uiso D U . . . . .
C19 C 0.544(4) 1.121(4) 0.153(2) 0.131(19) 1.0000 Uiso D U . . . . .
C20 C 0.598(4) 1.224(6) 0.075(2) 0.131(19) 1.0000 Uiso D U . . . . .
C21 C 0.531(5) 1.262(4) 0.090(3) 0.131(19) 1.0000 Uiso D U . . . . .
C22 C 0.357(2) 1.389(5) 0.287(3) 0.112(16) 1.0000 Uiso D U . . . . .
C23 C 0.3234(19) 1.468(5) 0.152(6) 0.112(16) 1.0000 Uiso D U . . . . .
C24 C 0.357(2) 1.384(6) 0.133(4) 0.112(16) 1.0000 Uiso D U . . . . .
C101 C 0.314(7) 0.658(8) 0.714(9) 0.26(3) 1.0000 Uiso D U . . . . .
C102 C 0.441(7) 0.626(6) 0.648(10) 0.26(3) 1.0000 Uiso D U . . . . .
C103 C 0.363(5) 0.784(6) 0.622(10) 0.26(3) 1.0000 Uiso D U . . . . .
C104 C 0.169(4) 1.363(7) 0.197(9) 0.20(3) 1.0000 Uiso D U . . . . .
C201 C 0.066(6) 1.465(8) 0.105(6) 0.20(3) 1.0000 Uiso D U . . . . .
C202 C 0.037(6) 1.354(8) 0.246(8) 0.20(3) 1.0000 Uiso D U . . . . .
N1 N 0.317(3) 1.052(3) 0.390(3) 0.070(13) 1.0000 Uiso D U . . . . .
N2 N 0.404(3) 1.129(3) 0.320(2) 0.070(13) 1.0000 Uiso D U . . . . .
N3 N 0.183(5) 0.902(4) 0.4605(10) 0.14(2) 1.0000 Uiso D U . . . . .
N4 N 0.120(4) 0.770(6) 0.4951(11) 0.14(2) 1.0000 Uiso D U . . . . .
N5 N 0.152(5) 1.151(4) 0.442(3) 0.107(16) 1.0000 Uiso D U . . . . .
N6 N 0.057(3) 1.254(6) 0.457(3) 0.107(16) 1.0000 Uiso D U . . . . .
N7 N 0.146(2) 0.999(6) 0.264(4) 0.110(16) 1.0000 Uiso D U . . . . .
N8 N 0.082(4) 0.927(6) 0.125(5) 0.110(16) 1.0000 Uiso D U . . . . .
N9 N 0.108(5) 0.803(3) 0.706(3) 0.140(19) 1.0000 Uiso D U . . . . .
N10 N 0.185(4) 0.908(4) 0.805(5) 0.140(19) 1.0000 Uiso D U . . . . .
N11 N 0.300(4) 1.029(3) -0.016(3) 0.104(15) 1.0000 Uiso D U . . . . .
N12 N 0.341(4) 1.129(2) 0.111(4) 0.104(15) 1.0000 Uiso D U . . . . .
N13 N 0.608(3) 1.134(5) 0.115(3) 0.131(19) 1.0000 Uiso D U . . . . .
N14 N 0.495(3) 1.198(7) 0.139(3) 0.131(19) 1.0000 Uiso D U . . . . .
N15 N 0.3227(17) 1.472(4) 0.249(6) 0.112(16) 1.0000 Uiso D U . . . . .
N16 N 0.3785(14) 1.333(3) 0.218(6) 0.112(16) 1.0000 Uiso D U . . . . .
N17 N 0.370(5) 0.682(5) 0.650(6) 0.26(3) 1.0000 Uiso D U . . . . .
N18 N 0.091(4) 1.401(4) 0.194(5) 0.20(3) 1.0000 Uiso D U . . . . .
O1 O 0.158(6) 1.287(6) 0.227(7) 0.20(3) 1.0000 Uiso D U . . . . .
O2 O 0.419(6) 0.826(5) 0.615(8) 0.26(3) 1.0000 Uiso D U . . . . .
H11 H 0.2876 1.1592 0.2899 0.0843 1.0000 Uiso R . . . . . .
H21 H 0.4014 0.9645 0.4732 0.0843 1.0000 Uiso R . . . . . .
H31 H 0.4958 1.0496 0.3961 0.0842 1.0000 Uiso R . . . . . .
H41 H 0.0709 0.9036 0.4775 0.1640 1.0000 Uiso R . . . . . .
H51 H 0.2835 0.8270 0.4588 0.1640 1.0000 Uiso R . . . . . .
H61 H 0.2146 0.6819 0.4973 0.1640 1.0000 Uiso R . . . . . .
H71 H 0.0361 1.1201 0.3982 0.1269 1.0000 Uiso R . . . . . .
H81 H 0.1352 1.3593 0.5196 0.1269 1.0000 Uiso R . . . . . .
H91 H 0.2389 1.2453 0.5021 0.1269 1.0000 Uiso R . . . . . .
H101 H 0.1565 0.8561 0.2356 0.1311 1.0000 Uiso R . . . . . .
H111 H 0.0283 1.0521 0.0688 0.1312 1.0000 Uiso R . . . . . .
H121 H 0.0979 1.1317 0.2204 0.1312 1.0000 Uiso R . . . . . .
H131 H 0.2197 0.8321 0.6970 0.1674 1.0000 Uiso R . . . . . .
H141 H 0.0993 0.9414 0.8802 0.1673 1.0000 Uiso R . . . . . .
H151 H 0.0154 0.8260 0.7713 0.1674 1.0000 Uiso R . . . . . .
H161 H 0.4072 1.0925 0.0133 0.1245 1.0000 Uiso R . . . . . .
H171 H 0.2379 1.1181 0.1578 0.1245 1.0000 Uiso R . . . . . .
H181 H 0.1937 1.0078 0.0181 0.1245 1.0000 Uiso R . . . . . .
H191 H 0.5346 1.0645 0.1871 0.1614 1.0000 Uiso R . . . . . .
H201 H 0.6337 1.2545 0.0418 0.1614 1.0000 Uiso R . . . . . .
H211 H 0.5109 1.3242 0.0678 0.1614 1.0000 Uiso R . . . . . .
H221 H 0.3633 1.3731 0.3546 0.1346 1.0000 Uiso R . . . . . .
H231 H 0.3044 1.5156 0.1037 0.1347 1.0000 Uiso R . . . . . .
H241 H 0.3655 1.3625 0.0713 0.1347 1.0000 Uiso R . . . . . .
H1011 H 0.2724 0.7047 0.7027 0.3139 1.0000 Uiso R . . . . . .
H1012 H 0.3401 0.6597 0.7824 0.3139 1.0000 Uiso R . . . . . .
H1013 H 0.2930 0.5947 0.6977 0.3139 1.0000 Uiso R . . . . . .
H1021 H 0.4684 0.6550 0.6028 0.3140 1.0000 Uiso R . . . . . .
H1022 H 0.4740 0.6261 0.7133 0.3140 1.0000 Uiso R . . . . . .
H1023 H 0.4269 0.5611 0.6286 0.3140 1.0000 Uiso R . . . . . .
H2011 H 0.0152 1.4892 0.1039 0.2459 1.0000 Uiso R . . . . . .
H2012 H 0.1022 1.5175 0.1076 0.2459 1.0000 Uiso R . . . . . .
H2013 H 0.0656 1.4272 0.0465 0.2459 1.0000 Uiso R . . . . . .
H2021 H -0.0109 1.3899 0.2348 0.2460 1.0000 Uiso R . . . . . .
H2022 H 0.0598 1.3523 0.3149 0.2460 1.0000 Uiso R . . . . . .
H2023 H 0.0268 1.2894 0.2213 0.2460 1.0000 Uiso R . . . . . .
H1041 H 0.2159 1.3913 0.1795 0.2461 1.0000 Uiso R . . . . . .
H1031 H 0.3121 0.8170 0.6097 0.3139 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.157(15) 0.064(13) 0.132(16) 0.006(8) 0.075(14) 0.023(10)
Zn2 0.141(15) 0.083(15) 0.121(17) 0.020(8) 0.058(15) 0.010(9)
Zn3 0.146(15) 0.081(14) 0.106(16) -0.033(8) 0.043(14) -0.021(9)
Zn4 0.186(18) 0.082(15) 0.142(18) 0.019(8) 0.108(17) -0.009(10)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1032(3)
loop_
_oxford_twin_element_scale_factors
0.799(15)
0.201(15)
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
Zn1 . N1 . 2.03(4) yes
Zn1 . N3 . 2.02(5) yes
Zn1 . N5 . 2.07(5) yes
Zn1 . N7 . 1.97(5) yes
Zn2 . N8 4_565 2.13(7) yes
Zn2 . N6 2_576 2.04(6) yes
Zn2 . N4 . 1.94(5) yes
Zn2 . N9 . 2.02(6) yes
Zn3 . N13 2_676 2.12(5) yes
Zn3 . N15 4_575 2.00(6) yes
Zn3 . N11 1_556 1.99(5) yes
Zn3 . N10 . 1.98(6) yes
Zn4 . N2 . 1.84(4) yes
Zn4 . N12 . 1.92(5) yes
Zn4 . N14 . 1.82(5) yes
Zn4 . N16 . 2.09(5) yes
C1 . N1 . 1.346(8) yes
C1 . N2 . 1.346(8) yes
C1 . H11 . 0.950 no
C2 . C3 . 1.356(8) yes
C2 . N1 . 1.355(8) yes
C2 . H21 . 0.950 no
C3 . N2 . 1.350(8) yes
C3 . H31 . 0.950 no
C4 . N3 . 1.341(8) yes
C4 . N4 . 1.344(8) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.355(8) yes
C5 . N3 . 1.354(8) yes
C5 . H51 . 0.950 no
C6 . N4 . 1.352(8) yes
C6 . H61 . 0.950 no
C7 . N5 . 1.345(8) yes
C7 . N6 . 1.346(8) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.357(8) yes
C8 . N6 . 1.352(8) yes
C8 . H81 . 0.950 no
C9 . N5 . 1.353(8) yes
C9 . H91 . 0.950 no
C10 . N7 . 1.344(8) yes
C10 . N8 . 1.345(8) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.355(8) yes
C11 . N8 . 1.352(8) yes
C11 . H111 . 0.950 no
C12 . N7 . 1.353(8) yes
C12 . H121 . 0.950 no
C13 . N9 . 1.345(8) yes
C13 . N10 . 1.344(8) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.357(8) yes
C14 . N10 . 1.352(8) yes
C14 . H141 . 0.950 no
C15 . N9 . 1.351(8) yes
C15 . H151 . 0.950 no
C16 . N11 . 1.345(8) yes
C16 . N12 . 1.346(8) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.356(8) yes
C17 . N12 . 1.351(8) yes
C17 . H171 . 0.950 no
C18 . N11 . 1.351(8) yes
C18 . H181 . 0.950 no
C19 . N13 . 1.343(8) yes
C19 . N14 . 1.344(8) yes
C19 . H191 . 0.950 no
C20 . C21 . 1.357(8) yes
C20 . N13 . 1.353(8) yes
C20 . H201 . 0.950 no
C21 . N14 . 1.352(8) yes
C21 . H211 . 0.950 no
C22 . N15 . 1.344(8) yes
C22 . N16 . 1.345(8) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.356(8) yes
C23 . N15 . 1.351(8) yes
C23 . H231 . 0.950 no
C24 . N16 . 1.351(8) yes
C24 . H241 . 0.950 no
C101 . N17 . 1.498(8) yes
C101 . H1011 . 0.960 no
C101 . H1012 . 0.960 no
C101 . H1013 . 0.960 no
C102 . N17 . 1.471(8) yes
C102 . H1021 . 0.960 no
C102 . H1022 . 0.960 no
C102 . H1023 . 0.960 no
C103 . N17 . 1.460(8) yes
C103 . O2 . 1.160(8) yes
C103 . H1031 . 0.980 no
C104 . N18 . 1.459(8) yes
C104 . O1 . 1.162(8) yes
C104 . H1041 . 0.980 no
C201 . N18 . 1.498(8) yes
C201 . H2011 . 0.960 no
C201 . H2012 . 0.960 no
C201 . H2013 . 0.960 no
C202 . N18 . 1.468(8) yes
C202 . H2021 . 0.960 no
C202 . H2022 . 0.960 no
C202 . H2023 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Zn1 . N3 . 115(3) yes
N1 . Zn1 . N5 . 113(3) yes
N3 . Zn1 . N5 . 117(3) yes
N1 . Zn1 . N7 . 107.1(12) yes
N3 . Zn1 . N7 . 97(2) yes
N5 . Zn1 . N7 . 106(3) yes
N8 4_565 Zn2 . N6 2_576 111(3) yes
N8 4_565 Zn2 . N4 . 113(3) yes
N6 2_576 Zn2 . N4 . 113(2) yes
N8 4_565 Zn2 . N9 . 108(3) yes
N6 2_576 Zn2 . N9 . 112(3) yes
N4 . Zn2 . N9 . 99(3) yes
N13 2_676 Zn3 . N15 4_575 94(2) yes
N13 2_676 Zn3 . N11 1_556 104.2(15) yes
N15 4_575 Zn3 . N11 1_556 115(3) yes
N13 2_676 Zn3 . N10 . 125(2) yes
N15 4_575 Zn3 . N10 . 106(2) yes
N11 1_556 Zn3 . N10 . 113(3) yes
N2 . Zn4 . N12 . 100(2) yes
N2 . Zn4 . N14 . 136(3) yes
N12 . Zn4 . N14 . 98(3) yes
N2 . Zn4 . N16 . 106(3) yes
N12 . Zn4 . N16 . 105.2(19) yes
N14 . Zn4 . N16 . 107(3) yes
N1 . C1 . N2 . 112.8(6) yes
N1 . C1 . H11 . 123.5 no
N2 . C1 . H11 . 123.7 no
C3 . C2 . N1 . 109.2(6) yes
C3 . C2 . H21 . 125.3 no
N1 . C2 . H21 . 125.5 no
C2 . C3 . N2 . 109.1(6) yes
C2 . C3 . H31 . 125.6 no
N2 . C3 . H31 . 125.4 no
N3 . C4 . N4 . 112.7(6) yes
N3 . C4 . H41 . 124.1 no
N4 . C4 . H41 . 123.2 no
C6 . C5 . N3 . 109.0(6) yes
C6 . C5 . H51 . 125.9 no
N3 . C5 . H51 . 125.1 no
C5 . C6 . N4 . 109.0(6) yes
C5 . C6 . H61 . 125.1 no
N4 . C6 . H61 . 126.0 no
N5 . C7 . N6 . 112.7(6) yes
N5 . C7 . H71 . 125.2 no
N6 . C7 . H71 . 122.1 no
C9 . C8 . N6 . 109.1(6) yes
C9 . C8 . H81 . 123.9 no
N6 . C8 . H81 . 127.0 no
C8 . C9 . N5 . 109.0(6) yes
C8 . C9 . H91 . 127.1 no
N5 . C9 . H91 . 123.9 no
N7 . C10 . N8 . 112.9(7) yes
N7 . C10 . H101 . 123.3 no
N8 . C10 . H101 . 123.8 no
C12 . C11 . N8 . 109.0(6) yes
C12 . C11 . H111 . 125.8 no
N8 . C11 . H111 . 125.2 no
C11 . C12 . N7 . 109.3(6) yes
C11 . C12 . H121 . 125.1 no
N7 . C12 . H121 . 125.6 no
N9 . C13 . N10 . 112.8(6) yes
N9 . C13 . H131 . 123.7 no
N10 . C13 . H131 . 123.5 no
C15 . C14 . N10 . 109.1(6) yes
C15 . C14 . H141 . 125.3 no
N10 . C14 . H141 . 125.6 no
C14 . C15 . N9 . 109.0(6) yes
C14 . C15 . H151 . 125.6 no
N9 . C15 . H151 . 125.4 no
N11 . C16 . N12 . 112.7(6) yes
N11 . C16 . H161 . 123.8 no
N12 . C16 . H161 . 123.5 no
C18 . C17 . N12 . 109.1(6) yes
C18 . C17 . H171 . 125.3 no
N12 . C17 . H171 . 125.6 no
C17 . C18 . N11 . 109.1(6) yes
C17 . C18 . H181 . 125.6 no
N11 . C18 . H181 . 125.3 no
N13 . C19 . N14 . 113.2(6) yes
N13 . C19 . H191 . 123.4 no
N14 . C19 . H191 . 123.4 no
C21 . C20 . N13 . 109.2(6) yes
C21 . C20 . H201 . 125.4 no
N13 . C20 . H201 . 125.4 no
C20 . C21 . N14 . 109.1(6) yes
C20 . C21 . H211 . 125.4 no
N14 . C21 . H211 . 125.5 no
N15 . C22 . N16 . 112.6(6) yes
N15 . C22 . H221 . 122.1 no
N16 . C22 . H221 . 125.3 no
C24 . C23 . N15 . 109.0(6) yes
C24 . C23 . H231 . 123.9 no
N15 . C23 . H231 . 127.1 no
C23 . C24 . N16 . 109.0(6) yes
C23 . C24 . H241 . 127.1 no
N16 . C24 . H241 . 123.9 no
N17 . C101 . H1011 . 109.1 no
N17 . C101 . H1012 . 110.0 no
H1011 . C101 . H1012 . 109.5 no
N17 . C101 . H1013 . 109.3 no
H1011 . C101 . H1013 . 109.5 no
H1012 . C101 . H1013 . 109.5 no
N17 . C102 . H1021 . 109.9 no
N17 . C102 . H1022 . 109.2 no
H1021 . C102 . H1022 . 109.5 no
N17 . C102 . H1023 . 109.4 no
H1021 . C102 . H1023 . 109.5 no
H1022 . C102 . H1023 . 109.5 no
N17 . C103 . O2 . 118.0(8) yes
N17 . C103 . H1031 . 121.3 no
O2 . C103 . H1031 . 120.6 no
N18 . C104 . O1 . 96(6) yes
N18 . C104 . H1041 . 132.3 no
O1 . C104 . H1041 . 132.0 no
N18 . C201 . H2011 . 109.3 no
N18 . C201 . H2012 . 109.9 no
H2011 . C201 . H2012 . 109.5 no
N18 . C201 . H2013 . 109.3 no
H2011 . C201 . H2013 . 109.5 no
H2012 . C201 . H2013 . 109.5 no
N18 . C202 . H2021 . 109.7 no
N18 . C202 . H2022 . 109.1 no
H2021 . C202 . H2022 . 109.5 no
N18 . C202 . H2023 . 109.6 no
H2021 . C202 . H2023 . 109.5 no
H2022 . C202 . H2023 . 109.5 no
C2 . N1 . C1 . 104.3(5) yes
C2 . N1 . Zn1 . 140(4) yes
C1 . N1 . Zn1 . 115(4) yes
C3 . N2 . C1 . 104.6(5) yes
C3 . N2 . Zn4 . 137(4) yes
C1 . N2 . Zn4 . 115(4) yes
C5 . N3 . C4 . 104.6(6) yes
C5 . N3 . Zn1 . 123(7) yes
C4 . N3 . Zn1 . 130(7) yes
C6 . N4 . C4 . 104.7(6) yes
C6 . N4 . Zn2 . 128(6) yes
C4 . N4 . Zn2 . 117(6) yes
C9 . N5 . C7 . 104.6(6) yes
C9 . N5 . Zn1 . 130(6) yes
C7 . N5 . Zn1 . 125(6) yes
C8 . N6 . C7 . 104.6(6) yes
C8 . N6 . Zn2 2_576 144(6) yes
C7 . N6 . Zn2 2_576 110(6) yes
C12 . N7 . C10 . 104.3(6) yes
C12 . N7 . Zn1 . 123(7) yes
C10 . N7 . Zn1 . 133(7) yes
Zn2 4_564 N8 . C11 . 153(6) yes
Zn2 4_564 N8 . C10 . 100(7) yes
C11 . N8 . C10 . 104.5(8) yes
C15 . N9 . C13 . 104.6(6) yes
C15 . N9 . Zn2 . 124(6) yes
C13 . N9 . Zn2 . 130(6) yes
C14 . N10 . C13 . 104.4(6) yes
C14 . N10 . Zn3 . 140(6) yes
C13 . N10 . Zn3 . 115(6) yes
C18 . N11 . C16 . 104.6(6) yes
C18 . N11 . Zn3 1_554 125(5) yes
C16 . N11 . Zn3 1_554 130(5) yes
C17 . N12 . C16 . 104.6(6) yes
C17 . N12 . Zn4 . 132(5) yes
C16 . N12 . Zn4 . 122(5) yes
C20 . N13 . Zn3 2_676 128(6) yes
C20 . N13 . C19 . 104.2(5) yes
Zn3 2_676 N13 . C19 . 126(6) yes
C21 . N14 . C19 . 104.3(6) yes
C21 . N14 . Zn4 . 140(6) yes
C19 . N14 . Zn4 . 114(7) yes
C23 . N15 . C22 . 104.7(5) yes
C23 . N15 . Zn3 4_574 147(6) yes
C22 . N15 . Zn3 4_574 108(6) yes
C24 . N16 . C22 . 104.7(6) yes
C24 . N16 . Zn4 . 118(6) yes
C22 . N16 . Zn4 . 137(6) yes
C101 . N17 . C102 . 124.1(8) yes
C101 . N17 . C103 . 109.9(8) yes
C102 . N17 . C103 . 122.1(8) yes
C201 . N18 . C202 . 123.7(8) yes
C201 . N18 . C104 . 110.1(8) yes
C202 . N18 . C104 . 122.0(8) yes
# Attachment '- phaseII_206.cif'
data_phaseII_206
_database_code_depnum_ccdc_archive 'CCDC 828169'
#TrackingRef '- phaseII_206.cif'
_audit_creation_date 11-03-21
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title 'trial in P2(1)/c'
_chemical_name_systematic ?
_chemical_name_common ZIF-4
_chemical_formula_moiety 'C24 H24 N16 Zn4, 2(C3 H7 N O)'
# Given Formula = C40 H50 N18 O2.50 Zn1
# Dc = 1.70 Fooo = 1920.00 Mu = 7.80 M = 888.34
# Found Formula = C30 H38 N18 O2 Zn4
# Dc = 1.80 FOOO = 1920.00 Mu = 27.86 M = 944.27
_chemical_formula_sum 'C30 H38 N18 O2 Zn4'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure 2060
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 17.4068(18)
_cell_length_b 14.0783(17)
_cell_length_c 14.5050(17)
_cell_angle_alpha 90
_cell_angle_beta 101.853(9)
_cell_angle_gamma 90
_cell_volume 3478.8(7)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_int_tables_number 14
# 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 .
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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 0.0029 0.0015 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 0.0057 0.0031 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'
Zn 0.3006 1.3591 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 944.27
_cell_measurement_reflns_used 1051
_cell_measurement_theta_min 2.4
_cell_measurement_theta_max 16.6
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.1
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_max 0.2
_exptl_crystal_density_diffrn 1.803
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.786
# Sheldrick geometric approximatio 1.00 1.00
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min 1.0000
_exptl_absorpt_correction_T_max 1.0000
_diffrn_measurement_device_type Unknown
_diffrn_measurement_device Serial
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.68890
_diffrn_source synchrotron
_diffrn_measurement_method \w/2\q
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'USER DEFINED DATA COLLECTION'
_computing_cell_refinement 'USER DEFINED CELL REFINEMENT'
_computing_data_reduction 'USER DEFINED DATA REDUCTION'
_computing_structure_solution 'USER DEFINED 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_reflns_number 2252
_reflns_number_total 870
_diffrn_reflns_av_R_equivalents 0.055
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 870
# Theoretical number of reflections is about 3160
_diffrn_reflns_theta_min 1.819
_diffrn_reflns_theta_max 15.113
_diffrn_measured_fraction_theta_max 0.550
_diffrn_reflns_theta_full 11.637
_diffrn_measured_fraction_theta_full 0.635
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_limit_l_max 10
_reflns_limit_h_min -12
_reflns_limit_h_max 12
_reflns_limit_k_min 0
_reflns_limit_k_max 9
_reflns_limit_l_min 0
_reflns_limit_l_max 10
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.78
_refine_diff_density_max 1.05
# 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>-10.0\s(I)
_refine_ls_number_reflns 870
_refine_ls_number_restraints 230
_refine_ls_number_parameters 237
_oxford_refine_ls_R_factor_ref 0.1675
_refine_ls_wR_factor_ref 0.2896
_refine_ls_goodness_of_fit_ref 1.1616
_refine_ls_shift/su_max 0.0386197
_refine_ls_shift/su_mean 0.0032771
# The values computed from all data
_oxford_reflns_number_all 870
_refine_ls_R_factor_all 0.1675
_refine_ls_wR_factor_all 0.2896
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 749
_refine_ls_R_factor_gt 0.1528
_refine_ls_wR_factor_gt 0.2865
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
12.7 11.0 2.99
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
User-defined data collection reference
User defined data reduction
User defined cell refinement
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.2036(6) 1.0287(6) 0.3943(7) 0.0856 1.0000 Uani . . . . . . .
Zn2 Zn 0.0662(6) 0.7312(6) 0.5968(7) 0.0808 1.0000 Uani . . . . . . .
Zn3 Zn 0.2919(6) 0.9628(7) 0.8567(7) 0.0865 1.0000 Uani . . . . . . .
Zn4 Zn 0.4113(6) 1.1924(6) 0.2016(7) 0.0826 1.0000 Uani . . . . . . .
C1 C 0.317(2) 1.123(2) 0.329(2) 0.061(10) 1.0000 Uiso D U . . . . .
C2 C 0.381(3) 1.0214(17) 0.4236(17) 0.061(10) 1.0000 Uiso D U . . . . .
C3 C 0.4307(19) 1.064(3) 0.376(2) 0.061(10) 1.0000 Uiso D U . . . . .
C4 C 0.122(2) 0.875(4) 0.4817(16) 0.094(13) 1.0000 Uiso D U . . . . .
C5 C 0.240(2) 0.835(4) 0.4799(16) 0.094(13) 1.0000 Uiso D U . . . . .
C6 C 0.204(3) 0.761(3) 0.5129(13) 0.094(13) 1.0000 Uiso D U . . . . .
C7 C 0.070(3) 1.160(3) 0.4054(15) 0.076(11) 1.0000 Uiso D U . . . . .
C8 C 0.115(3) 1.285(2) 0.4818(17) 0.076(11) 1.0000 Uiso D U . . . . .
C9 C 0.176(2) 1.228(3) 0.4750(18) 0.076(11) 1.0000 Uiso D U . . . . .
C10 C 0.139(2) 0.906(4) 0.232(4) 0.089(11) 1.0000 Uiso D U . . . . .
C11 C 0.0740(15) 0.982(5) 0.115(3) 0.089(11) 1.0000 Uiso D U . . . . .
C12 C 0.102(2) 1.045(3) 0.185(4) 0.089(11) 1.0000 Uiso D U . . . . .
C13 C 0.180(3) 0.860(3) 0.737(3) 0.106(13) 1.0000 Uiso D U . . . . .
C14 C 0.120(3) 0.893(2) 0.847(3) 0.106(13) 1.0000 Uiso D U . . . . .
C15 C 0.073(2) 0.837(3) 0.783(4) 0.106(13) 1.0000 Uiso D U . . . . .
C16 C 0.356(2) 1.083(2) 0.021(3) 0.081(11) 1.0000 Uiso D U . . . . .
C17 C 0.271(3) 1.092(2) 0.107(3) 0.081(11) 1.0000 Uiso D U . . . . .
C18 C 0.2405(19) 1.039(2) 0.030(3) 0.081(11) 1.0000 Uiso D U . . . . .
C19 C 0.559(3) 1.119(3) 0.175(2) 0.108(13) 1.0000 Uiso D U . . . . .
C20 C 0.599(3) 1.201(4) 0.071(2) 0.108(13) 1.0000 Uiso D U . . . . .
C21 C 0.532(3) 1.241(2) 0.088(3) 0.108(13) 1.0000 Uiso D U . . . . .
C22 C 0.3391(12) 1.366(3) 0.280(2) 0.076(11) 1.0000 Uiso D U . . . . .
C23 C 0.3286(12) 1.467(3) 0.169(3) 0.076(11) 1.0000 Uiso D U . . . . .
C24 C 0.3573(11) 1.386(4) 0.140(2) 0.076(11) 1.0000 Uiso D U . . . . .
C101 C 0.329(5) 0.647(7) 0.730(7) 0.24(2) 1.0000 Uiso D U . . . . .
C102 C 0.467(5) 0.618(5) 0.689(7) 0.24(2) 1.0000 Uiso D U . . . . .
C103 C 0.372(4) 0.750(6) 0.618(7) 0.24(2) 1.0000 Uiso D U . . . . .
C104 C 0.167(5) 1.345(7) 0.194(8) 0.21(2) 1.0000 Uiso D U . . . . .
C201 C 0.075(5) 1.457(6) 0.103(5) 0.21(2) 1.0000 Uiso D U . . . . .
C202 C 0.036(5) 1.370(6) 0.246(6) 0.21(2) 1.0000 Uiso D U . . . . .
N1 N 0.308(2) 1.058(3) 0.394(2) 0.060(10) 1.0000 Uiso D U . . . . .
N2 N 0.391(3) 1.129(2) 0.3162(19) 0.061(10) 1.0000 Uiso D U . . . . .
N3 N 0.189(3) 0.908(3) 0.4597(11) 0.094(13) 1.0000 Uiso D U . . . . .
N4 N 0.129(3) 0.786(4) 0.5144(13) 0.094(13) 1.0000 Uiso D U . . . . .
N5 N 0.149(3) 1.148(3) 0.427(2) 0.076(11) 1.0000 Uiso D U . . . . .
N6 N 0.047(2) 1.242(4) 0.438(2) 0.076(11) 1.0000 Uiso D U . . . . .
N7 N 0.1435(17) 0.998(5) 0.260(3) 0.089(11) 1.0000 Uiso D U . . . . .
N8 N 0.097(2) 0.894(3) 0.145(5) 0.089(11) 1.0000 Uiso D U . . . . .
N9 N 0.110(4) 0.8154(19) 0.713(3) 0.106(13) 1.0000 Uiso D U . . . . .
N10 N 0.188(3) 0.908(2) 0.818(4) 0.106(13) 1.0000 Uiso D U . . . . .
N11 N 0.294(3) 1.0329(18) -0.025(2) 0.081(11) 1.0000 Uiso D U . . . . .
N12 N 0.344(3) 1.1196(16) 0.102(3) 0.081(11) 1.0000 Uiso D U . . . . .
N13 N 0.616(2) 1.123(3) 0.126(3) 0.108(13) 1.0000 Uiso D U . . . . .
N14 N 0.5064(19) 1.190(4) 0.154(3) 0.108(13) 1.0000 Uiso D U . . . . .
N15 N 0.3169(8) 1.456(3) 0.257(3) 0.076(11) 1.0000 Uiso D U . . . . .
N16 N 0.3642(9) 1.321(2) 0.210(3) 0.076(11) 1.0000 Uiso D U . . . . .
N17 N 0.389(4) 0.662(4) 0.671(4) 0.24(2) 1.0000 Uiso D U . . . . .
N18 N 0.094(4) 1.398(4) 0.191(4) 0.21(2) 1.0000 Uiso D U . . . . .
O1 O 0.174(5) 1.280(5) 0.244(6) 0.21(2) 1.0000 Uiso D U . . . . .
O2 O 0.425(5) 0.797(5) 0.609(6) 0.24(2) 1.0000 Uiso D U . . . . .
H11 H 0.2755 1.1616 0.2951 0.0698 1.0000 Uiso R . . . . . .
H21 H 0.3931 0.9726 0.4695 0.0698 1.0000 Uiso R . . . . . .
H31 H 0.4851 1.0500 0.3855 0.0699 1.0000 Uiso R . . . . . .
H41 H 0.0754 0.9117 0.4772 0.1068 1.0000 Uiso R . . . . . .
H51 H 0.2921 0.8362 0.4696 0.1068 1.0000 Uiso R . . . . . .
H61 H 0.2275 0.7015 0.5307 0.1068 1.0000 Uiso R . . . . . .
H71 H 0.0364 1.1109 0.3758 0.0863 1.0000 Uiso R . . . . . .
H81 H 0.1164 1.3470 0.5071 0.0863 1.0000 Uiso R . . . . . .
H91 H 0.2294 1.2452 0.4975 0.0863 1.0000 Uiso R . . . . . .
H101 H 0.1578 0.8506 0.2669 0.1077 1.0000 Uiso R . . . . . .
H111 H 0.0460 1.0055 0.0560 0.1078 1.0000 Uiso R . . . . . .
H121 H 0.0991 1.1124 0.1873 0.1078 1.0000 Uiso R . . . . . .
H131 H 0.2160 0.8564 0.6964 0.1164 1.0000 Uiso R . . . . . .
H141 H 0.1109 0.9186 0.9046 0.1165 1.0000 Uiso R . . . . . .
H151 H 0.0224 0.8172 0.7920 0.1165 1.0000 Uiso R . . . . . .
H161 H 0.4043 1.0896 0.0001 0.0948 1.0000 Uiso R . . . . . .
H171 H 0.2432 1.1087 0.1548 0.0947 1.0000 Uiso R . . . . . .
H181 H 0.1900 1.0108 0.0161 0.0948 1.0000 Uiso R . . . . . .
H191 H 0.5568 1.0719 0.2211 0.1308 1.0000 Uiso R . . . . . .
H201 H 0.6281 1.2239 0.0270 0.1309 1.0000 Uiso R . . . . . .
H211 H 0.5069 1.2957 0.0571 0.1308 1.0000 Uiso R . . . . . .
H221 H 0.3377 1.3362 0.3381 0.0857 1.0000 Uiso R . . . . . .
H231 H 0.3188 1.5248 0.1341 0.0858 1.0000 Uiso R . . . . . .
H241 H 0.3693 1.3764 0.0796 0.0858 1.0000 Uiso R . . . . . .
H1011 H 0.2822 0.6806 0.7029 0.2844 1.0000 Uiso R . . . . . .
H1012 H 0.3527 0.6753 0.7895 0.2844 1.0000 Uiso R . . . . . .
H1013 H 0.3160 0.5817 0.7409 0.2844 1.0000 Uiso R . . . . . .
H1021 H 0.4928 0.6292 0.6379 0.2844 1.0000 Uiso R . . . . . .
H1022 H 0.4981 0.6444 0.7461 0.2844 1.0000 Uiso R . . . . . .
H1023 H 0.4614 0.5507 0.6975 0.2844 1.0000 Uiso R . . . . . .
H2011 H 0.0258 1.4882 0.1006 0.2202 1.0000 Uiso R . . . . . .
H2012 H 0.1153 1.5033 0.1025 0.2202 1.0000 Uiso R . . . . . .
H2013 H 0.0712 1.4157 0.0496 0.2202 1.0000 Uiso R . . . . . .
H2021 H -0.0089 1.4106 0.2326 0.2202 1.0000 Uiso R . . . . . .
H2022 H 0.0594 1.3732 0.3121 0.2202 1.0000 Uiso R . . . . . .
H2023 H 0.0203 1.3054 0.2301 0.2202 1.0000 Uiso R . . . . . .
H1041 H 0.2094 1.3695 0.1661 0.2204 1.0000 Uiso R . . . . . .
H1031 H 0.3243 0.7497 0.5686 0.2845 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.126(11) 0.035(9) 0.109(11) 0.004(5) 0.054(9) 0.004(6)
Zn2 0.109(10) 0.018(8) 0.123(12) 0.005(5) 0.041(9) -0.004(6)
Zn3 0.108(10) 0.057(8) 0.100(12) -0.004(6) 0.034(9) -0.013(7)
Zn4 0.109(10) 0.036(9) 0.113(12) 0.001(5) 0.046(9) -0.002(6)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1042(2)
loop_
_oxford_twin_element_scale_factors
0.756
0.244
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
Zn1 . N1 . 1.86(3) yes
Zn1 . N3 . 1.99(4) yes
Zn1 . N5 . 2.04(3) yes
Zn1 . N7 . 2.06(4) yes
Zn2 . N6 2_576 1.97(4) yes
Zn2 . N8 4_565 1.93(4) yes
Zn2 . N4 . 1.94(3) yes
Zn2 . N9 . 2.08(4) yes
Zn3 . N13 2_676 1.98(4) yes
Zn3 . N11 1_556 1.97(4) yes
Zn3 . N15 4_575 1.96(3) yes
Zn3 . N10 . 1.94(4) yes
Zn4 . N2 . 1.98(3) yes
Zn4 . N12 . 1.95(4) yes
Zn4 . N14 . 1.92(4) yes
Zn4 . N16 . 2.00(3) yes
C1 . N1 . 1.344(8) yes
C1 . N2 . 1.347(8) yes
C1 . H11 . 0.950 no
C2 . C3 . 1.357(8) yes
C2 . N1 . 1.354(8) yes
C2 . H21 . 0.950 no
C3 . N2 . 1.351(8) yes
C3 . H31 . 0.950 no
C4 . N3 . 1.343(8) yes
C4 . N4 . 1.343(8) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.357(8) yes
C5 . N3 . 1.353(8) yes
C5 . H51 . 0.950 no
C6 . N4 . 1.351(8) yes
C6 . H61 . 0.950 no
C7 . N5 . 1.346(8) yes
C7 . N6 . 1.347(8) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.358(8) yes
C8 . N6 . 1.353(8) yes
C8 . H81 . 0.950 no
C9 . N5 . 1.354(8) yes
C9 . H91 . 0.950 no
C10 . N7 . 1.344(8) yes
C10 . N8 . 1.343(8) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.355(8) yes
C11 . N8 . 1.352(8) yes
C11 . H111 . 0.950 no
C12 . N7 . 1.355(8) yes
C12 . H121 . 0.950 no
C13 . N9 . 1.345(8) yes
C13 . N10 . 1.344(8) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.357(8) yes
C14 . N10 . 1.352(8) yes
C14 . H141 . 0.950 no
C15 . N9 . 1.349(8) yes
C15 . H151 . 0.950 no
C16 . N11 . 1.345(8) yes
C16 . N12 . 1.344(8) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.356(8) yes
C17 . N12 . 1.353(8) yes
C17 . H171 . 0.950 no
C18 . N11 . 1.352(8) yes
C18 . H181 . 0.950 no
C19 . N13 . 1.340(8) yes
C19 . N14 . 1.343(8) yes
C19 . H191 . 0.950 no
C20 . C21 . 1.357(8) yes
C20 . N13 . 1.354(8) yes
C20 . H201 . 0.950 no
C21 . N14 . 1.349(8) yes
C21 . H211 . 0.950 no
C22 . N15 . 1.342(8) yes
C22 . N16 . 1.343(8) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.356(8) yes
C23 . N15 . 1.349(8) yes
C23 . H231 . 0.950 no
C24 . N16 . 1.350(8) yes
C24 . H241 . 0.950 no
C101 . N17 . 1.499(9) yes
C101 . H1011 . 0.960 no
C101 . H1012 . 0.960 no
C101 . H1013 . 0.960 no
C102 . N17 . 1.470(9) yes
C102 . H1021 . 0.960 no
C102 . H1022 . 0.960 no
C102 . H1023 . 0.960 no
C103 . N17 . 1.459(9) yes
C103 . O2 . 1.158(9) yes
C103 . H1031 . 0.980 no
C104 . N18 . 1.458(9) yes
C104 . O1 . 1.162(9) yes
C104 . H1041 . 0.980 no
C201 . N18 . 1.498(9) yes
C201 . H2011 . 0.960 no
C201 . H2012 . 0.960 no
C201 . H2013 . 0.960 no
C202 . N18 . 1.467(9) yes
C202 . H2021 . 0.960 no
C202 . H2022 . 0.960 no
C202 . H2023 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Zn1 . N3 . 115(2) yes
N1 . Zn1 . N5 . 108.5(19) yes
N3 . Zn1 . N5 . 118.7(16) yes
N1 . Zn1 . N7 . 110.6(10) yes
N3 . Zn1 . N7 . 100.3(18) yes
N5 . Zn1 . N7 . 103(2) yes
N6 2_576 Zn2 . N8 4_565 117.2(18) yes
N6 2_576 Zn2 . N4 . 115.3(18) yes
N8 4_565 Zn2 . N4 . 116(2) yes
N6 2_576 Zn2 . N9 . 106(2) yes
N8 4_565 Zn2 . N9 . 101(2) yes
N4 . Zn2 . N9 . 96.7(18) yes
N13 2_676 Zn3 . N11 1_556 109.1(13) yes
N13 2_676 Zn3 . N15 4_575 99(2) yes
N11 1_556 Zn3 . N15 4_575 112(2) yes
N13 2_676 Zn3 . N10 . 118.3(15) yes
N11 1_556 Zn3 . N10 . 107(2) yes
N15 4_575 Zn3 . N10 . 110.7(15) yes
N2 . Zn4 . N12 . 101.5(15) yes
N2 . Zn4 . N14 . 128(2) yes
N12 . Zn4 . N14 . 98.8(18) yes
N2 . Zn4 . N16 . 102.2(19) yes
N12 . Zn4 . N16 . 109.1(12) yes
N14 . Zn4 . N16 . 116(2) yes
N1 . C1 . N2 . 112.9(6) yes
N1 . C1 . H11 . 124.7 no
N2 . C1 . H11 . 122.4 no
C3 . C2 . N1 . 109.1(6) yes
C3 . C2 . H21 . 126.5 no
N1 . C2 . H21 . 124.3 no
C2 . C3 . N2 . 109.1(6) yes
C2 . C3 . H31 . 124.3 no
N2 . C3 . H31 . 126.6 no
N3 . C4 . N4 . 112.8(6) yes
N3 . C4 . H41 . 124.4 no
N4 . C4 . H41 . 122.8 no
C6 . C5 . N3 . 108.9(6) yes
C6 . C5 . H51 . 126.3 no
N3 . C5 . H51 . 124.7 no
C5 . C6 . N4 . 109.1(6) yes
C5 . C6 . H61 . 124.7 no
N4 . C6 . H61 . 126.3 no
N5 . C7 . N6 . 112.8(6) yes
N5 . C7 . H71 . 121.4 no
N6 . C7 . H71 . 125.5 no
C9 . C8 . N6 . 109.2(6) yes
C9 . C8 . H81 . 127.5 no
N6 . C8 . H81 . 123.1 no
C8 . C9 . N5 . 109.0(6) yes
C8 . C9 . H91 . 123.4 no
N5 . C9 . H91 . 127.5 no
N7 . C10 . N8 . 113.1(7) yes
N7 . C10 . H101 . 129.8 no
N8 . C10 . H101 . 117.0 no
C12 . C11 . N8 . 109.0(7) yes
C12 . C11 . H111 . 119.1 no
N8 . C11 . H111 . 131.8 no
C11 . C12 . N7 . 109.2(6) yes
C11 . C12 . H121 . 131.8 no
N7 . C12 . H121 . 118.9 no
N9 . C13 . N10 . 112.9(6) yes
N9 . C13 . H131 . 120.1 no
N10 . C13 . H131 . 127.0 no
C15 . C14 . N10 . 109.2(6) yes
C15 . C14 . H141 . 128.9 no
N10 . C14 . H141 . 121.9 no
C14 . C15 . N9 . 109.0(6) yes
C14 . C15 . H151 . 122.1 no
N9 . C15 . H151 . 128.9 no
N11 . C16 . N12 . 112.6(6) yes
N11 . C16 . H161 . 124.4 no
N12 . C16 . H161 . 123.0 no
C18 . C17 . N12 . 109.0(6) yes
C18 . C17 . H171 . 124.8 no
N12 . C17 . H171 . 126.2 no
C17 . C18 . N11 . 109.1(6) yes
C17 . C18 . H181 . 126.1 no
N11 . C18 . H181 . 124.8 no
N13 . C19 . N14 . 113.3(6) yes
N13 . C19 . H191 . 123.0 no
N14 . C19 . H191 . 123.7 no
C21 . C20 . N13 . 109.2(6) yes
C21 . C20 . H201 . 125.0 no
N13 . C20 . H201 . 125.8 no
C20 . C21 . N14 . 109.0(6) yes
C20 . C21 . H211 . 125.8 no
N14 . C21 . H211 . 125.1 no
N15 . C22 . N16 . 112.7(6) yes
N15 . C22 . H221 . 124.8 no
N16 . C22 . H221 . 122.5 no
C24 . C23 . N15 . 109.1(6) yes
C24 . C23 . H231 . 126.6 no
N15 . C23 . H231 . 124.3 no
C23 . C24 . N16 . 108.9(6) yes
C23 . C24 . H241 . 124.4 no
N16 . C24 . H241 . 126.7 no
N17 . C101 . H1011 . 108.6 no
N17 . C101 . H1012 . 103.1 no
H1011 . C101 . H1012 . 109.5 no
N17 . C101 . H1013 . 116.4 no
H1011 . C101 . H1013 . 109.5 no
H1012 . C101 . H1013 . 109.5 no
N17 . C102 . H1021 . 110.5 no
N17 . C102 . H1022 . 108.9 no
H1021 . C102 . H1022 . 109.5 no
N17 . C102 . H1023 . 109.0 no
H1021 . C102 . H1023 . 109.5 no
H1022 . C102 . H1023 . 109.5 no
N17 . C103 . O2 . 118.1(9) yes
N17 . C103 . H1031 . 115.3 no
O2 . C103 . H1031 . 119.5 no
N18 . C104 . O1 . 114(6) yes
N18 . C104 . H1041 . 122.2 no
O1 . C104 . H1041 . 122.7 no
N18 . C201 . H2011 . 109.2 no
N18 . C201 . H2012 . 110.7 no
H2011 . C201 . H2012 . 109.5 no
N18 . C201 . H2013 . 108.5 no
H2011 . C201 . H2013 . 109.5 no
H2012 . C201 . H2013 . 109.5 no
N18 . C202 . H2021 . 110.5 no
N18 . C202 . H2022 . 109.5 no
H2021 . C202 . H2022 . 109.5 no
N18 . C202 . H2023 . 108.4 no
H2021 . C202 . H2023 . 109.5 no
H2022 . C202 . H2023 . 109.5 no
C2 . N1 . C1 . 104.4(6) yes
C2 . N1 . Zn1 . 140(3) yes
C1 . N1 . Zn1 . 114(3) yes
C3 . N2 . C1 . 104.5(6) yes
C3 . N2 . Zn4 . 134(3) yes
C1 . N2 . Zn4 . 119(3) yes
C5 . N3 . C4 . 104.6(6) yes
C5 . N3 . Zn1 . 127(4) yes
C4 . N3 . Zn1 . 128(4) yes
C6 . N4 . C4 . 104.6(6) yes
C6 . N4 . Zn2 . 125(4) yes
C4 . N4 . Zn2 . 125(4) yes
C9 . N5 . C7 . 104.6(6) yes
C9 . N5 . Zn1 . 132(4) yes
C7 . N5 . Zn1 . 123(4) yes
C8 . N6 . C7 . 104.5(6) yes
C8 . N6 . Zn2 2_576 140(4) yes
C7 . N6 . Zn2 2_576 115(4) yes
C12 . N7 . C10 . 104.2(6) yes
C12 . N7 . Zn1 . 138(5) yes
C10 . N7 . Zn1 . 118(5) yes
C11 . N8 . C10 . 104.5(8) yes
C11 . N8 . Zn2 4_564 133(5) yes
C10 . N8 . Zn2 4_564 121(5) yes
C15 . N9 . C13 . 104.6(6) yes
C15 . N9 . Zn2 . 126(4) yes
C13 . N9 . Zn2 . 129(4) yes
C14 . N10 . C13 . 104.4(6) yes
C14 . N10 . Zn3 . 143(4) yes
C13 . N10 . Zn3 . 112(4) yes
C18 . N11 . C16 . 104.6(6) yes
C18 . N11 . Zn3 1_554 131(4) yes
C16 . N11 . Zn3 1_554 124(4) yes
C17 . N12 . C16 . 104.7(6) yes
C17 . N12 . Zn4 . 123(4) yes
C16 . N12 . Zn4 . 132(4) yes
C20 . N13 . C19 . 104.1(6) yes
C20 . N13 . Zn3 2_676 130(4) yes
C19 . N13 . Zn3 2_676 125(4) yes
C21 . N14 . C19 . 104.4(6) yes
C21 . N14 . Zn4 . 133(4) yes
C19 . N14 . Zn4 . 122(4) yes
C23 . N15 . C22 . 104.6(6) yes
C23 . N15 . Zn3 4_574 137(4) yes
C22 . N15 . Zn3 4_574 118(4) yes
C24 . N16 . C22 . 104.6(6) yes
C24 . N16 . Zn4 . 123(3) yes
C22 . N16 . Zn4 . 132(3) yes
C101 . N17 . C102 . 124.2(8) yes
C101 . N17 . C103 . 110.0(8) yes
C102 . N17 . C103 . 122.3(8) yes
C201 . N18 . C202 . 123.9(8) yes
C201 . N18 . C104 . 110.5(8) yes
C202 . N18 . C104 . 122.3(8) yes
# Attachment '- phaseII_321.cif'
data_phaseII_321
_database_code_depnum_ccdc_archive 'CCDC 828170'
#TrackingRef '- phaseII_321.cif'
_audit_creation_date 11-03-21
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title 'phase2 in P2(1)/c'
_chemical_name_systematic ?
_chemical_name_common ZIF-4
_chemical_formula_moiety 'C24 H24 N16 Zn4, 2(C3 H7 N O)'
# Given Formula = C38 H40 N10 O2 Zn4
# Dc = 1.84 Fooo = 1920.00 Mu = 28.85 M = 930.32
# Found Formula = C30 H38 N18 O2 Zn4
# Dc = 1.87 FOOO = 1920.00 Mu = 28.93 M = 944.27
_chemical_formula_sum 'C30 H38 N18 O2 Zn4'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description colourless
_exptl_crystal_colour block
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure 3210
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.44
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6].. 16.97 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 14.60 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.53
088_ALERT_3_A Poor Data / Parameter Ratio .................... 3.51
201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 40
341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 68
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.424 1252
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 289
909_ALERT_3_G Percentage of Observed Data at Theta(Max) ...... 31.58
All of the above are caused by shading from the pressure cell. 1,2 and 1,3
restraints were applied to all non-hydrogen distances.
413_ALERT_2_A Short Inter XH3 .. XHn H2023 .. H151 .. 1.79 Ang.
432_ALERT_2_A Short Inter X...Y Contact C19 .. C103 .. 2.84 Ang.
411_ALERT_2_B Short Inter H...H Contact H51 .. H201 .. 1.91 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2011 .. H71 .. 2.05 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2012 .. H41 .. 2.09 Ang.
432_ALERT_2_B Short Inter X...Y Contact N14 .. C103 .. 2.87 Ang.
411_ALERT_2_C Short Inter H...H Contact H111 .. H111 .. 2.10 Ang.
413_ALERT_2_C Short Inter XH3 .. XHn H2011 .. H41 .. 2.10 Ang.
432_ALERT_2_C Short Inter X...Y Contact O2 .. C3 .. 2.94 Ang.
432_ALERT_2_C Short Inter X...Y Contact C4 .. C201 .. 3.12 Ang.
432_ALERT_2_C Short Inter X...Y Contact C7 .. C201 .. 3.11 Ang.
432_ALERT_2_C Short Inter X...Y Contact C9 .. C104 .. 3.12 Ang.
432_ALERT_2_C Short Inter X...Y Contact C22 .. C104 .. 3.19 Ang.
Short contacts are expected at high-pressure.
082_ALERT_2_C High R1 Value .................................. 0.15
084_ALERT_2_C High R2 Value .................................. 0.30
The sample has undergone a phase transition which caused the crystal to
'break up', increasing the R1 value and increasing e.s.d's on measured
unit cell dimensions.
731_ALERT_1_A Bond Calc 1.35(9), Rep 1.342(8) ...... 9.90 su-Ra
C4 -N3 1.555 1.555
731_ALERT_1_A Bond Calc 1.33(9), Rep 1.344(8) ...... 9.90 su-Ra
C4 -N4 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(8), Rep 1.356(8) ...... 9.90 su-Ra
C5 -C6 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.354(8) ...... 9.90 su-Ra
C5 -N3 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(9), Rep 1.353(8) ...... 9.90 su-Ra
C6 -N4 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(9), Rep 1.345(8) ...... 9.90 su-Ra
C7 -N5 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.346(8) ...... 8.75 su-Ra
C7 -N6 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.358(8) ...... 8.75 su-Ra
C8 -C9 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.353(8) ...... 9.90 su-Ra
C8 -N6 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(8), Rep 1.345(8) ...... 9.90 su-Ra
C10 -N7 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(8), Rep 1.345(8) ...... 9.90 su-Ra
C10 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.356(8) ...... 8.75 su-Ra
C11 -C12 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(9), Rep 1.351(8) ...... 9.90 su-Ra
C11 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.353(8) ...... 8.75 su-Ra
C12 -N7 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.345(8) ...... 8.75 su-Ra
C13 -N9 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.350(8) ...... 8.75 su-Ra
C15 -N9 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.352(8) ...... 8.75 su-Ra
C17 -N12 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.344(8) ...... 8.75 su-Ra
C19 -N14 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.357(8) ...... 8.75 su-Ra
C20 -C21 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.353(8) ...... 8.75 su-Ra
C20 -N13 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.351(8) ...... 8.75 su-Ra
C21 -N14 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(8), Rep 1.344(8) ...... 9.90 su-Ra
C22 -N15 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.344(8) ...... 8.75 su-Ra
C22 -N16 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.356(8) ...... 8.75 su-Ra
C23 -C24 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.351(8) ...... 9.90 su-Ra
C23 -N15 1.555 1.555
731_ALERT_1_A Bond Calc 1.37(8), Rep 1.353(8) ...... 9.90 su-Ra
C24 -N16 1.555 1.555
731_ALERT_1_A Bond Calc 1.50(10), Rep 1.498(8) ...... 9.90 su-Ra
C101 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(10), Rep 1.471(8) ...... 9.90 su-Ra
C102 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(8), Rep 1.460(8) ...... 9.90 su-Ra
C103 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(12), Rep 1.160(8) ...... 9.90 su-Ra
C103 -O2 1.555 1.555
731_ALERT_1_A Bond Calc 1.45(9), Rep 1.459(8) ...... 9.90 su-Ra
C104 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(12), Rep 1.162(8) ...... 9.90 su-Ra
C104 -O1 1.555 1.555
731_ALERT_1_A Bond Calc 1.50(9), Rep 1.498(8) ...... 9.90 su-Ra
C201 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(9), Rep 1.467(8) ...... 9.90 su-Ra
C202 -N18 1.555 1.555
732_ALERT_1_A Angle Calc 112(5), Rep 112.8(6) ...... 8.33 su-Ra
N3 -C4 -N4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(5), Rep 109.3(6) ...... 8.33 su-Ra
C11 -C12 -N7 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 118(7), Rep 118.0(8) ...... 8.75 su-Ra
N17 -C103 -O2 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.6(6) ...... 8.33 su-Ra
C5 -N3 -C4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.7(6) ...... 8.33 su-Ra
C6 -N4 -C4 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 105(5), Rep 104.6(6) ...... 8.33 su-Ra
C8 -N6 -C7 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 122(7), Rep 122.0(8) ...... 8.75 su-Ra
C102 -N17 -C103 1.555 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(5), Rep 1.346(8) ...... 6.25 su-Ra
C1 -N1 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.345(8) ...... 7.50 su-Ra
C1 -N2 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.355(8) ...... 7.50 su-Ra
C2 -C3 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.354(8) ...... 7.50 su-Ra
C2 -N1 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.352(8) ...... 6.25 su-Ra
C3 -N2 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.354(8) ...... 7.50 su-Ra
C9 -N5 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(5), Rep 1.343(8) ...... 6.25 su-Ra
C13 -N10 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.358(8) ...... 7.50 su-Ra
C14 -C15 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.352(8) ...... 7.50 su-Ra
C14 -N10 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.346(8) ...... 6.25 su-Ra
C16 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.345(8) ...... 7.50 su-Ra
C16 -N12 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.356(8) ...... 7.50 su-Ra
C17 -C18 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.351(8) ...... 7.50 su-Ra
C18 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.342(8) ...... 7.50 su-Ra
C19 -N13 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.8(6) ...... 5.00 su-Ra
N1 -C1 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C3 -C2 -N1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.1(6) ...... 6.67 su-Ra
C2 -C3 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C6 -C5 -N3 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 108.9(6) ...... 6.67 su-Ra
C5 -C6 -N4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.7(6) ...... 6.67 su-Ra
N5 -C7 -N6 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.1(6) ...... 6.67 su-Ra
C9 -C8 -N6 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 108.9(6) ...... 6.67 su-Ra
C8 -C9 -N5 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(5), Rep 112.9(7) ...... 7.14 su-Ra
N7 -C10 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 108(4), Rep 109.0(7) ...... 5.71 su-Ra
C12 -C11 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.9(6) ...... 6.67 su-Ra
N9 -C13 -N10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.2(6) ...... 5.00 su-Ra
C15 -C14 -N10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(4), Rep 109.0(6) ...... 6.67 su-Ra
C14 -C15 -N9 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 112(4), Rep 112.6(6) ...... 6.67 su-Ra
N11 -C16 -N12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.1(6) ...... 6.67 su-Ra
C18 -C17 -N12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(4), Rep 109.1(6) ...... 6.67 su-Ra
C17 -C18 -N11 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 114(4), Rep 113.3(6) ...... 6.67 su-Ra
N13 -C19 -N14 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.2(6) ...... 6.67 su-Ra
C21 -C20 -N13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.1(6) ...... 6.67 su-Ra
C20 -C21 -N14 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.6(6) ...... 6.67 su-Ra
N15 -C22 -N16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C24 -C23 -N15 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C23 -C24 -N16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.4(6) ...... 5.00 su-Ra
C2 -N1 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.5(6) ...... 5.00 su-Ra
C3 -N2 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.6(6) ...... 6.67 su-Ra
C9 -N5 -C7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.3(6) ...... 6.67 su-Ra
C12 -N7 -C10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(8) ...... 5.00 su-Ra
C11 -N8 -C10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(6) ...... 5.00 su-Ra
C15 -N9 -C13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.4(6) ...... 6.67 su-Ra
C14 -N10 -C13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(6) ...... 5.00 su-Ra
C18 -N11 -C16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(6) ...... 6.67 su-Ra
C17 -N12 -C16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.1(6) ...... 6.67 su-Ra
C20 -N13 -C19 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.3(6) ...... 6.67 su-Ra
C21 -N14 -C19 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.7(6) ...... 6.67 su-Ra
C23 -N15 -C22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.6(6) ...... 6.67 su-Ra
C24 -N16 -C22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 124(6), Rep 124.1(8) ...... 7.50 su-Ra
C101 -N17 -C102 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(6), Rep 109.9(8) ...... 7.50 su-Ra
C101 -N17 -C103 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 123(6), Rep 123.6(8) ...... 7.50 su-Ra
C201 -N18 -C202 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 111(6), Rep 110.2(8) ...... 7.50 su-Ra
C201 -N18 -C104 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 122(6), Rep 121.8(8) ...... 7.50 su-Ra
C202 -N18 -C104 1.555 1.555 1.555
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 is badly in error.
152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 500 Ang.
These are caused by rounding errors.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C101
092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.69 Ang.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
These are correct.
720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 14
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
919_ALERT_3_B Reflection(s) # Likely Affected by the Beamstop 1
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 17.450(5)
_cell_length_b 13.912(5)
_cell_length_c 14.118(5)
_cell_angle_alpha 90
_cell_angle_beta 102.18(3)
_cell_angle_gamma 90
_cell_volume 3350.1(18)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_int_tables_number 14
# 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 .
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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 0.0029 0.0015 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 0.0057 0.0031 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 0.0101 0.0057 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'
Zn 0.3006 1.3591 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 944.27
_cell_measurement_reflns_used 846
_cell_measurement_theta_min 3
_cell_measurement_theta_max 17
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.140
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_max 0.220
_exptl_crystal_density_diffrn 1.872
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.893
# Sheldrick geometric approximatio 0.61 0.67
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.36
_exptl_absorpt_correction_T_max 0.67
_diffrn_measurement_device_type Unknown
_diffrn_measurement_device Serial
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.68890
_diffrn_source synchrotron
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'USER DEFINED DATA COLLECTION'
_computing_cell_refinement 'USER DEFINED CELL REFINEMENT'
_computing_data_reduction 'USER DEFINED DATA REDUCTION'
_computing_structure_solution 'USER DEFINED 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_reflns_number 926
_reflns_number_total 926
_diffrn_reflns_av_R_equivalents 0.087
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 926
# Theoretical number of reflections is about 4271
_diffrn_reflns_theta_min 1.831
_diffrn_reflns_theta_max 16.973
_diffrn_measured_fraction_theta_max 0.436
_diffrn_reflns_theta_full 14.596
_diffrn_measured_fraction_theta_full 0.529
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -14
_reflns_limit_h_max 13
_reflns_limit_k_min 0
_reflns_limit_k_max 10
_reflns_limit_l_min 0
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.77
_refine_diff_density_max 0.85
# 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>-10.0\s(I)
_refine_ls_number_reflns 835
_refine_ls_number_restraints 289
_refine_ls_number_parameters 238
_oxford_refine_ls_R_factor_ref 0.1879
_refine_ls_wR_factor_ref 0.3048
_refine_ls_goodness_of_fit_ref 1.0450
_refine_ls_shift/su_max 0.0175478
_refine_ls_shift/su_mean 0.0014590
# The values computed from all data
_oxford_reflns_number_all 835
_refine_ls_R_factor_all 0.1879
_refine_ls_wR_factor_all 0.3048
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 606
_refine_ls_R_factor_gt 0.1513
_refine_ls_wR_factor_gt 0.2836
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
16.9 17.0 5.83
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
User-defined data collection reference
User defined data reduction
User defined cell refinement
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.2055(6) 1.0291(7) 0.3997(8) 0.0912 1.0000 Uani . U . . . . .
Zn2 Zn 0.0635(6) 0.7239(6) 0.5924(8) 0.0927 1.0000 Uani . U . . . . .
Zn3 Zn 0.2924(6) 0.9574(7) 0.8590(8) 0.1017 1.0000 Uani . U . . . . .
Zn4 Zn 0.4145(6) 1.1932(7) 0.2062(8) 0.0958 1.0000 Uani . U . . . . .
C1 C 0.328(2) 1.126(2) 0.335(2) 0.072(10) 1.0000 Uiso D U . . . . .
C2 C 0.384(3) 1.0142(19) 0.4278(17) 0.072(10) 1.0000 Uiso D U . . . . .
C3 C 0.4379(19) 1.057(3) 0.386(2) 0.072(10) 1.0000 Uiso D U . . . . .
C4 C 0.120(3) 0.873(5) 0.4777(12) 0.115(15) 1.0000 Uiso D U . . . . .
C5 C 0.238(2) 0.838(5) 0.4713(11) 0.115(15) 1.0000 Uiso D U . . . . .
C6 C 0.201(4) 0.757(3) 0.4917(11) 0.115(15) 1.0000 Uiso D U . . . . .
C7 C 0.072(3) 1.158(3) 0.4117(16) 0.098(12) 1.0000 Uiso D U . . . . .
C8 C 0.113(4) 1.287(3) 0.4878(19) 0.098(12) 1.0000 Uiso D U . . . . .
C9 C 0.176(2) 1.231(4) 0.483(2) 0.098(12) 1.0000 Uiso D U . . . . .
C10 C 0.132(2) 0.909(3) 0.217(5) 0.095(12) 1.0000 Uiso D U . . . . .
C11 C 0.0650(16) 1.008(5) 0.117(3) 0.095(12) 1.0000 Uiso D U . . . . .
C12 C 0.103(2) 1.057(3) 0.196(4) 0.095(12) 1.0000 Uiso D U . . . . .
C13 C 0.175(3) 0.845(2) 0.727(3) 0.098(12) 1.0000 Uiso D U . . . . .
C14 C 0.118(3) 0.891(2) 0.838(2) 0.098(12) 1.0000 Uiso D U . . . . .
C15 C 0.067(2) 0.839(2) 0.773(4) 0.098(12) 1.0000 Uiso D U . . . . .
C16 C 0.355(2) 1.082(2) 0.024(3) 0.085(11) 1.0000 Uiso D U . . . . .
C17 C 0.268(3) 1.092(2) 0.109(3) 0.085(11) 1.0000 Uiso D U . . . . .
C18 C 0.238(2) 1.042(2) 0.028(4) 0.085(11) 1.0000 Uiso D U . . . . .
C19 C 0.556(3) 1.113(3) 0.1669(19) 0.120(15) 1.0000 Uiso D U . . . . .
C20 C 0.600(3) 1.215(4) 0.0804(18) 0.120(15) 1.0000 Uiso D U . . . . .
C21 C 0.534(3) 1.251(3) 0.103(3) 0.120(15) 1.0000 Uiso D U . . . . .
C22 C 0.3503(15) 1.370(4) 0.285(3) 0.106(14) 1.0000 Uiso D U . . . . .
C23 C 0.3280(13) 1.469(3) 0.167(4) 0.106(14) 1.0000 Uiso D U . . . . .
C24 C 0.3564(15) 1.387(5) 0.136(3) 0.106(14) 1.0000 Uiso D U . . . . .
C101 C 0.314(4) 0.648(6) 0.714(7) 0.20(2) 1.0000 Uiso D U . . . . .
C102 C 0.453(4) 0.616(5) 0.677(7) 0.20(2) 1.0000 Uiso D U . . . . .
C103 C 0.386(5) 0.780(4) 0.662(8) 0.20(2) 1.0000 Uiso D U . . . . .
C104 C 0.169(4) 1.350(6) 0.187(7) 0.181(18) 1.0000 Uiso D U . . . . .
C201 C 0.071(5) 1.459(6) 0.099(5) 0.181(18) 1.0000 Uiso D U . . . . .
C202 C 0.039(4) 1.358(6) 0.241(6) 0.181(18) 1.0000 Uiso D U . . . . .
N1 N 0.314(2) 1.058(3) 0.396(2) 0.072(10) 1.0000 Uiso D U . . . . .
N2 N 0.403(3) 1.128(2) 0.3267(19) 0.072(10) 1.0000 Uiso D U . . . . .
N3 N 0.187(4) 0.912(3) 0.4623(9) 0.115(15) 1.0000 Uiso D U . . . . .
N4 N 0.127(3) 0.779(4) 0.4962(9) 0.115(15) 1.0000 Uiso D U . . . . .
N5 N 0.151(4) 1.149(3) 0.435(2) 0.098(12) 1.0000 Uiso D U . . . . .
N6 N 0.047(3) 1.242(4) 0.443(3) 0.098(12) 1.0000 Uiso D U . . . . .
N7 N 0.1453(17) 0.996(5) 0.261(3) 0.095(12) 1.0000 Uiso D U . . . . .
N8 N 0.083(3) 0.914(4) 0.130(4) 0.095(12) 1.0000 Uiso D U . . . . .
N9 N 0.102(3) 0.8091(17) 0.702(3) 0.098(12) 1.0000 Uiso D U . . . . .
N10 N 0.187(2) 0.896(2) 0.809(3) 0.098(12) 1.0000 Uiso D U . . . . .
N11 N 0.292(3) 1.0343(17) -0.027(2) 0.085(11) 1.0000 Uiso D U . . . . .
N12 N 0.342(3) 1.1179(16) 0.108(3) 0.085(11) 1.0000 Uiso D U . . . . .
N13 N 0.615(2) 1.127(4) 0.121(3) 0.120(15) 1.0000 Uiso D U . . . . .
N14 N 0.505(2) 1.186(5) 0.158(3) 0.120(15) 1.0000 Uiso D U . . . . .
N15 N 0.3238(11) 1.459(4) 0.261(4) 0.106(14) 1.0000 Uiso D U . . . . .
N16 N 0.3709(10) 1.323(3) 0.211(5) 0.106(14) 1.0000 Uiso D U . . . . .
N17 N 0.383(4) 0.676(4) 0.672(4) 0.20(2) 1.0000 Uiso D U . . . . .
N18 N 0.095(3) 1.397(4) 0.187(4) 0.181(18) 1.0000 Uiso D U . . . . .
O1 O 0.163(4) 1.287(5) 0.239(6) 0.181(18) 1.0000 Uiso D U . . . . .
O2 O 0.431(4) 0.812(4) 0.621(6) 0.20(2) 1.0000 Uiso D U . . . . .
H11 H 0.2891 1.1689 0.3014 0.0867 1.0000 Uiso R . . . . . .
H21 H 0.3934 0.9622 0.4723 0.0866 1.0000 Uiso R . . . . . .
H31 H 0.4917 1.0394 0.3961 0.0867 1.0000 Uiso R . . . . . .
H41 H 0.0735 0.9089 0.4759 0.1377 1.0000 Uiso R . . . . . .
H51 H 0.2908 0.8416 0.4644 0.1378 1.0000 Uiso R . . . . . .
H61 H 0.2244 0.6946 0.5012 0.1379 1.0000 Uiso R . . . . . .
H71 H 0.0384 1.1107 0.3771 0.1172 1.0000 Uiso R . . . . . .
H81 H 0.1156 1.3483 0.5179 0.1173 1.0000 Uiso R . . . . . .
H91 H 0.2295 1.2470 0.5094 0.1172 1.0000 Uiso R . . . . . .
H101 H 0.1543 0.8511 0.2462 0.1136 1.0000 Uiso R . . . . . .
H111 H 0.0314 1.0348 0.0620 0.1138 1.0000 Uiso R . . . . . .
H121 H 0.0994 1.1249 0.2050 0.1137 1.0000 Uiso R . . . . . .
H131 H 0.2137 0.8357 0.6892 0.1166 1.0000 Uiso R . . . . . .
H141 H 0.1080 0.9201 0.8953 0.1167 1.0000 Uiso R . . . . . .
H151 H 0.0141 0.8251 0.7773 0.1167 1.0000 Uiso R . . . . . .
H161 H 0.4028 1.0885 0.0027 0.1013 1.0000 Uiso R . . . . . .
H171 H 0.2413 1.1073 0.1597 0.1012 1.0000 Uiso R . . . . . .
H181 H 0.1861 1.0155 0.0123 0.1012 1.0000 Uiso R . . . . . .
H191 H 0.5509 1.0560 0.2027 0.1439 1.0000 Uiso R . . . . . .
H201 H 0.6311 1.2468 0.0420 0.1439 1.0000 Uiso R . . . . . .
H211 H 0.5110 1.3116 0.0827 0.1439 1.0000 Uiso R . . . . . .
H221 H 0.3542 1.3427 0.3472 0.1279 1.0000 Uiso R . . . . . .
H231 H 0.3132 1.5252 0.1287 0.1279 1.0000 Uiso R . . . . . .
H241 H 0.3648 1.3759 0.0729 0.1279 1.0000 Uiso R . . . . . .
H1011 H 0.2755 0.6981 0.7019 0.2415 1.0000 Uiso R . . . . . .
H1012 H 0.3315 0.6389 0.7825 0.2415 1.0000 Uiso R . . . . . .
H1013 H 0.2922 0.5895 0.6844 0.2415 1.0000 Uiso R . . . . . .
H1021 H 0.4891 0.6481 0.6448 0.2416 1.0000 Uiso R . . . . . .
H1022 H 0.4777 0.6046 0.7433 0.2416 1.0000 Uiso R . . . . . .
H1023 H 0.4384 0.5552 0.6453 0.2416 1.0000 Uiso R . . . . . .
H2011 H 0.0220 1.4895 0.1000 0.2172 1.0000 Uiso R . . . . . .
H2012 H 0.1107 1.5075 0.0998 0.2172 1.0000 Uiso R . . . . . .
H2013 H 0.0664 1.4206 0.0420 0.2172 1.0000 Uiso R . . . . . .
H2021 H -0.0067 1.3984 0.2326 0.2175 1.0000 Uiso R . . . . . .
H2022 H 0.0628 1.3545 0.3091 0.2175 1.0000 Uiso R . . . . . .
H2023 H 0.0235 1.2944 0.2178 0.2175 1.0000 Uiso R . . . . . .
H1041 H 0.2117 1.3668 0.1541 0.2175 1.0000 Uiso R . . . . . .
H1031 H 0.3490 0.8219 0.6865 0.2417 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.141(8) 0.028(6) 0.127(6) -0.006(5) 0.081(6) -0.006(6)
Zn2 0.126(8) 0.030(7) 0.139(10) 0.006(5) 0.065(6) -0.006(5)
Zn3 0.149(9) 0.049(8) 0.127(6) -0.006(5) 0.075(6) -0.020(6)
Zn4 0.136(9) 0.039(7) 0.135(8) 0.000(5) 0.081(8) -0.003(6)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1197(3)
loop_
_oxford_twin_element_scale_factors
0.791(12)
0.209(12)
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
Zn1 . N1 . 1.94(3) yes
Zn1 . N3 . 1.91(4) yes
Zn1 . N5 . 2.04(4) yes
Zn1 . N7 . 2.08(4) yes
Zn2 . N8 4_565 2.00(5) yes
Zn2 . N6 2_576 1.95(4) yes
Zn2 . N4 . 2.07(4) yes
Zn2 . N9 . 1.95(4) yes
Zn3 . N13 2_676 1.97(4) yes
Zn3 . N15 4_575 1.97(4) yes
Zn3 . N11 1_556 1.94(4) yes
Zn3 . N10 . 2.01(4) yes
Zn4 . N2 . 1.97(3) yes
Zn4 . N12 . 1.97(4) yes
Zn4 . N14 . 1.85(4) yes
Zn4 . N16 . 1.97(4) yes
C1 . N1 . 1.346(8) yes
C1 . N2 . 1.345(8) yes
C1 . H11 . 0.950 no
C2 . C3 . 1.355(8) yes
C2 . N1 . 1.354(8) yes
C2 . H21 . 0.950 no
C3 . N2 . 1.352(8) yes
C3 . H31 . 0.950 no
C4 . N3 . 1.342(8) yes
C4 . N4 . 1.344(8) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.356(8) yes
C5 . N3 . 1.354(8) yes
C5 . H51 . 0.950 no
C6 . N4 . 1.353(8) yes
C6 . H61 . 0.950 no
C7 . N5 . 1.345(8) yes
C7 . N6 . 1.346(8) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.358(8) yes
C8 . N6 . 1.353(8) yes
C8 . H81 . 0.950 no
C9 . N5 . 1.354(8) yes
C9 . H91 . 0.950 no
C10 . N7 . 1.345(8) yes
C10 . N8 . 1.345(8) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.356(8) yes
C11 . N8 . 1.351(8) yes
C11 . H111 . 0.950 no
C12 . N7 . 1.353(8) yes
C12 . H121 . 0.950 no
C13 . N9 . 1.345(8) yes
C13 . N10 . 1.343(8) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.358(8) yes
C14 . N10 . 1.352(8) yes
C14 . H141 . 0.950 no
C15 . N9 . 1.350(8) yes
C15 . H151 . 0.950 no
C16 . N11 . 1.346(8) yes
C16 . N12 . 1.345(8) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.356(8) yes
C17 . N12 . 1.352(8) yes
C17 . H171 . 0.950 no
C18 . N11 . 1.351(8) yes
C18 . H181 . 0.950 no
C19 . N13 . 1.342(8) yes
C19 . N14 . 1.344(8) yes
C19 . H191 . 0.950 no
C20 . C21 . 1.357(8) yes
C20 . N13 . 1.353(8) yes
C20 . H201 . 0.950 no
C21 . N14 . 1.351(8) yes
C21 . H211 . 0.950 no
C22 . N15 . 1.344(8) yes
C22 . N16 . 1.344(8) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.356(8) yes
C23 . N15 . 1.351(8) yes
C23 . H231 . 0.950 no
C24 . N16 . 1.353(8) yes
C24 . H241 . 0.950 no
C101 . N17 . 1.498(8) yes
C101 . H1011 . 0.960 no
C101 . H1012 . 0.960 no
C101 . H1013 . 0.960 no
C102 . N17 . 1.471(8) yes
C102 . H1021 . 0.960 no
C102 . H1022 . 0.960 no
C102 . H1023 . 0.960 no
C103 . N17 . 1.460(8) yes
C103 . O2 . 1.160(8) yes
C103 . H1031 . 0.980 no
C104 . N18 . 1.459(8) yes
C104 . O1 . 1.162(8) yes
C104 . H1041 . 0.980 no
C201 . N18 . 1.498(8) yes
C201 . H2011 . 0.960 no
C201 . H2012 . 0.960 no
C201 . H2013 . 0.960 no
C202 . N18 . 1.467(8) yes
C202 . H2021 . 0.960 no
C202 . H2022 . 0.960 no
C202 . H2023 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Zn1 . N3 . 117(3) yes
N1 . Zn1 . N5 . 110(2) yes
N3 . Zn1 . N5 . 116.7(20) yes
N1 . Zn1 . N7 . 108.9(9) yes
N3 . Zn1 . N7 . 98.3(16) yes
N5 . Zn1 . N7 . 104(2) yes
N8 4_565 Zn2 . N6 2_576 114(2) yes
N8 4_565 Zn2 . N4 . 116(2) yes
N6 2_576 Zn2 . N4 . 112.2(19) yes
N8 4_565 Zn2 . N9 . 111(2) yes
N6 2_576 Zn2 . N9 . 102(3) yes
N4 . Zn2 . N9 . 99.0(19) yes
N13 2_676 Zn3 . N15 4_575 96(2) yes
N13 2_676 Zn3 . N11 1_556 110.9(13) yes
N15 4_575 Zn3 . N11 1_556 108(2) yes
N13 2_676 Zn3 . N10 . 117.1(17) yes
N15 4_575 Zn3 . N10 . 111.9(18) yes
N11 1_556 Zn3 . N10 . 111(2) yes
N2 . Zn4 . N12 . 101.5(14) yes
N2 . Zn4 . N14 . 123(3) yes
N12 . Zn4 . N14 . 100.3(18) yes
N2 . Zn4 . N16 . 107(2) yes
N12 . Zn4 . N16 . 108.5(13) yes
N14 . Zn4 . N16 . 115(3) yes
N1 . C1 . N2 . 112.8(6) yes
N1 . C1 . H11 . 123.6 no
N2 . C1 . H11 . 123.7 no
C3 . C2 . N1 . 109.1(6) yes
C3 . C2 . H21 . 125.4 no
N1 . C2 . H21 . 125.5 no
C2 . C3 . N2 . 109.1(6) yes
C2 . C3 . H31 . 125.5 no
N2 . C3 . H31 . 125.4 no
N3 . C4 . N4 . 112.8(6) yes
N3 . C4 . H41 . 123.7 no
N4 . C4 . H41 . 123.5 no
C6 . C5 . N3 . 109.0(6) yes
C6 . C5 . H51 . 125.6 no
N3 . C5 . H51 . 125.4 no
C5 . C6 . N4 . 108.9(6) yes
C5 . C6 . H61 . 125.4 no
N4 . C6 . H61 . 125.7 no
N5 . C7 . N6 . 112.7(6) yes
N5 . C7 . H71 . 123.5 no
N6 . C7 . H71 . 123.7 no
C9 . C8 . N6 . 109.1(6) yes
C9 . C8 . H81 . 125.5 no
N6 . C8 . H81 . 125.3 no
C8 . C9 . N5 . 108.9(6) yes
C8 . C9 . H91 . 125.4 no
N5 . C9 . H91 . 125.6 no
N7 . C10 . N8 . 112.9(7) yes
N7 . C10 . H101 . 123.3 no
N8 . C10 . H101 . 123.8 no
C12 . C11 . N8 . 109.0(7) yes
C12 . C11 . H111 . 125.7 no
N8 . C11 . H111 . 125.3 no
C11 . C12 . N7 . 109.3(6) yes
C11 . C12 . H121 . 125.2 no
N7 . C12 . H121 . 125.6 no
N9 . C13 . N10 . 112.9(6) yes
N9 . C13 . H131 . 123.5 no
N10 . C13 . H131 . 123.6 no
C15 . C14 . N10 . 109.2(6) yes
C15 . C14 . H141 . 125.5 no
N10 . C14 . H141 . 125.4 no
C14 . C15 . N9 . 109.0(6) yes
C14 . C15 . H151 . 125.5 no
N9 . C15 . H151 . 125.6 no
N11 . C16 . N12 . 112.6(6) yes
N11 . C16 . H161 . 123.6 no
N12 . C16 . H161 . 123.8 no
C18 . C17 . N12 . 109.1(6) yes
C18 . C17 . H171 . 125.5 no
N12 . C17 . H171 . 125.4 no
C17 . C18 . N11 . 109.1(6) yes
C17 . C18 . H181 . 125.4 no
N11 . C18 . H181 . 125.5 no
N13 . C19 . N14 . 113.3(6) yes
N13 . C19 . H191 . 123.3 no
N14 . C19 . H191 . 123.4 no
C21 . C20 . N13 . 109.2(6) yes
C21 . C20 . H201 . 125.3 no
N13 . C20 . H201 . 125.4 no
C20 . C21 . N14 . 109.1(6) yes
C20 . C21 . H211 . 125.5 no
N14 . C21 . H211 . 125.4 no
N15 . C22 . N16 . 112.6(6) yes
N15 . C22 . H221 . 123.9 no
N16 . C22 . H221 . 123.4 no
C24 . C23 . N15 . 109.0(6) yes
C24 . C23 . H231 . 125.8 no
N15 . C23 . H231 . 125.2 no
C23 . C24 . N16 . 109.0(6) yes
C23 . C24 . H241 . 125.2 no
N16 . C24 . H241 . 125.7 no
N17 . C101 . H1011 . 109.8 no
N17 . C101 . H1012 . 109.0 no
H1011 . C101 . H1012 . 109.5 no
N17 . C101 . H1013 . 109.5 no
H1011 . C101 . H1013 . 109.5 no
H1012 . C101 . H1013 . 109.5 no
N17 . C102 . H1021 . 109.1 no
N17 . C102 . H1022 . 109.2 no
H1021 . C102 . H1022 . 109.5 no
N17 . C102 . H1023 . 110.1 no
H1021 . C102 . H1023 . 109.5 no
H1022 . C102 . H1023 . 109.5 no
N17 . C103 . O2 . 118.0(8) yes
N17 . C103 . H1031 . 120.9 no
O2 . C103 . H1031 . 121.0 no
N18 . C104 . O1 . 98(5) yes
N18 . C104 . H1041 . 130.9 no
O1 . C104 . H1041 . 131.3 no
N18 . C201 . H2011 . 109.5 no
N18 . C201 . H2012 . 109.3 no
H2011 . C201 . H2012 . 109.5 no
N18 . C201 . H2013 . 109.6 no
H2011 . C201 . H2013 . 109.5 no
H2012 . C201 . H2013 . 109.5 no
N18 . C202 . H2021 . 109.6 no
N18 . C202 . H2022 . 109.8 no
H2021 . C202 . H2022 . 109.5 no
N18 . C202 . H2023 . 109.0 no
H2021 . C202 . H2023 . 109.5 no
H2022 . C202 . H2023 . 109.5 no
C2 . N1 . C1 . 104.4(6) yes
C2 . N1 . Zn1 . 136(3) yes
C1 . N1 . Zn1 . 118(3) yes
C3 . N2 . C1 . 104.5(6) yes
C3 . N2 . Zn4 . 139(3) yes
C1 . N2 . Zn4 . 111(3) yes
C5 . N3 . C4 . 104.6(6) yes
C5 . N3 . Zn1 . 121(5) yes
C4 . N3 . Zn1 . 131(5) yes
C6 . N4 . C4 . 104.7(6) yes
C6 . N4 . Zn2 . 127(4) yes
C4 . N4 . Zn2 . 117(4) yes
C9 . N5 . C7 . 104.6(6) yes
C9 . N5 . Zn1 . 134(4) yes
C7 . N5 . Zn1 . 122(4) yes
C8 . N6 . C7 . 104.6(6) yes
C8 . N6 . Zn2 2_576 135(5) yes
C7 . N6 . Zn2 2_576 120(5) yes
C12 . N7 . C10 . 104.3(6) yes
C12 . N7 . Zn1 . 126(5) yes
C10 . N7 . Zn1 . 129(5) yes
C11 . N8 . C10 . 104.6(8) yes
C11 . N8 . Zn2 4_564 151(5) yes
C10 . N8 . Zn2 4_564 104(5) yes
C15 . N9 . C13 . 104.6(6) yes
C15 . N9 . Zn2 . 130(4) yes
C13 . N9 . Zn2 . 125(4) yes
C14 . N10 . C13 . 104.4(6) yes
C14 . N10 . Zn3 . 136(4) yes
C13 . N10 . Zn3 . 120(4) yes
C18 . N11 . C16 . 104.6(6) yes
C18 . N11 . Zn3 1_554 130(4) yes
C16 . N11 . Zn3 1_554 124(4) yes
C17 . N12 . C16 . 104.6(6) yes
C17 . N12 . Zn4 . 127(4) yes
C16 . N12 . Zn4 . 129(4) yes
C20 . N13 . C19 . 104.1(6) yes
C20 . N13 . Zn3 2_676 133(5) yes
C19 . N13 . Zn3 2_676 122(5) yes
C21 . N14 . C19 . 104.3(6) yes
C21 . N14 . Zn4 . 129(5) yes
C19 . N14 . Zn4 . 127(5) yes
C23 . N15 . C22 . 104.7(6) yes
C23 . N15 . Zn3 4_574 135(5) yes
C22 . N15 . Zn3 4_574 120(5) yes
C24 . N16 . C22 . 104.6(6) yes
C24 . N16 . Zn4 . 126(5) yes
C22 . N16 . Zn4 . 130(5) yes
C101 . N17 . C102 . 124.1(8) yes
C101 . N17 . C103 . 109.9(8) yes
C102 . N17 . C103 . 122.0(8) yes
C201 . N18 . C202 . 123.6(8) yes
C201 . N18 . C104 . 110.2(8) yes
C202 . N18 . C104 . 121.8(8) yes
# Attachment '- phaseII_56.cif'
data_phaseII_56
_database_code_depnum_ccdc_archive 'CCDC 828171'
#TrackingRef '- phaseII_56.cif'
_audit_creation_date 11-03-21
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title '1to4 in P2(1)/c'
_chemical_name_systematic ?
_chemical_name_common ZIF-4
_chemical_formula_moiety 'C24 H24 N16 Zn4, 2(C3 H7 N O)'
# Given Formula = C20 H20 N16 O3 Zn2
# Dc = 1.18 Fooo = 1920.00 Mu = 13.23 M = 663.24
# Found Formula = C30 H38 N18 O2 Zn4
# Dc = 1.68 FOOO = 1920.00 Mu = 25.90 M = 944.27
_chemical_formula_sum 'C30 H38 N18 O2 Zn4'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure 560
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.70
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6].. 15.71 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 12.10 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.75
088_ALERT_3_A Poor Data / Parameter Ratio .................... 2.54
201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 40
341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 56
910_ALERT_3_B Missing # of FCF Reflections Below Th(Min) ..... 11
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.381 535
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 7
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 287
All of the above are caused by shading from the pressure cell. 1,2 and 1,3
restraints were applied to all non-hydrogen distamces.
082_ALERT_2_C High R1 Value .................................. 0.14
The sample has undergone a phase transition which caused the crystal to
'break up', increasing the R1 value.
411_ALERT_2_C Short Inter H...H Contact H111 .. H331 .. 2.12 Ang.
411_ALERT_2_B Short Inter H...H Contact H111 .. H321 .. 1.97 Ang.
432_ALERT_2_B Short Inter X...Y Contact C11 .. C32 .. 2.98 Ang.
432_ALERT_2_B Short Inter X...Y Contact C11 .. C33 .. 3.06 Ang.
Short contacts are expected at high-pressure.
731_ALERT_1_A Bond Calc 1.46(9), Rep 1.460(8) ...... 9.90 su-Ra
C1 -N1 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(10), Rep 1.161(8) ...... 9.90 su-Ra
C1 -O1 1.555 1.555
731_ALERT_1_A Bond Calc 1.45(11), Rep 1.459(8) ...... 9.90 su-Ra
C11 -N10 1.555 1.555
731_ALERT_1_A Bond Calc 1.17(11), Rep 1.159(8) ...... 9.90 su-Ra
C11 -O2 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.344(8) ...... 8.75 su-Ra
C21 -N20 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.343(8) ...... 8.75 su-Ra
C21 -N22 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.346(8) ...... 8.75 su-Ra
C25 -N24 1.555 1.555
731_ALERT_1_A Bond Calc 1.34(7), Rep 1.358(8) ...... 8.75 su-Ra
C27 -C28 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.353(8) ...... 8.75 su-Ra
C27 -N26 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.352(8) ...... 8.75 su-Ra
C39 -N22 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.352(8) ...... 8.75 su-Ra
C40 -N20 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(9), Rep 1.468(8) ...... 9.90 su-Ra
C111 -N1 1.555 1.555
731_ALERT_1_A Bond Calc 1.51(9), Rep 1.499(8) ...... 9.90 su-Ra
C112 -N1 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(12), Rep 1.470(8) ...... 9.90 su-Ra
C121 -N10 1.555 1.555
731_ALERT_1_A Bond Calc 1.51(13), Rep 1.500(8) ...... 9.90 su-Ra
C122 -N10 1.555 1.555
732_ALERT_1_A Angle Calc 118(7), Rep 118.1(8) ...... 8.75 su-Ra
N1 -C1 -O1 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 117(7), Rep 117.9(8) ...... 8.75 su-Ra
N10 -C11 -O2 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 123(7), Rep 124.0(8) ...... 8.75 su-Ra
C122 -N10 -C121 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 110(7), Rep 109.8(8) ...... 8.75 su-Ra
C122 -N10 -C11 1.555 1.555 1.555
732_ALERT_1_A Angle Calc 123(7), Rep 121.9(8) ...... 8.75 su-Ra
C121 -N10 -C11 1.555 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(5), Rep 1.345(8) ...... 6.25 su-Ra
C3 -N2 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.344(8) ...... 7.50 su-Ra
C3 -N4 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(5), Rep 1.342(8) ...... 6.25 su-Ra
C7 -N6 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.344(8) ...... 6.25 su-Ra
C7 -N8 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.357(8) ...... 6.25 su-Ra
C9 -C10 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(4), Rep 1.352(8) ...... 5.00 su-Ra
C9 -N8 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.353(8) ...... 6.25 su-Ra
C10 -N6 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.345(8) ...... 6.25 su-Ra
C12 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.346(8) ...... 7.50 su-Ra
C12 -N13 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.356(8) ...... 6.25 su-Ra
C14 -C15 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.352(8) ...... 7.50 su-Ra
C14 -N13 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.352(8) ...... 7.50 su-Ra
C15 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.344(8) ...... 7.50 su-Ra
C17 -N16 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.345(8) ...... 7.50 su-Ra
C17 -N18 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.346(8) ...... 7.50 su-Ra
C25 -N26 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.354(8) ...... 6.25 su-Ra
C28 -N24 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.343(8) ...... 7.50 su-Ra
C30 -N29 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.344(8) ...... 7.50 su-Ra
C30 -N31 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.357(8) ...... 7.50 su-Ra
C32 -C33 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.352(8) ...... 7.50 su-Ra
C32 -N31 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.353(8) ...... 7.50 su-Ra
C33 -N29 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(4), Rep 1.345(8) ...... 5.00 su-Ra
C35 -N34 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.345(8) ...... 7.50 su-Ra
C35 -N36 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.356(8) ...... 6.25 su-Ra
C37 -C38 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.352(8) ...... 6.25 su-Ra
C37 -N36 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.353(8) ...... 7.50 su-Ra
C38 -N34 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.356(8) ...... 7.50 su-Ra
C39 -C40 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.357(8) ...... 6.25 su-Ra
C41 -C42 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.351(8) ...... 7.50 su-Ra
C41 -N18 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.352(8) ...... 7.50 su-Ra
C42 -N16 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.356(8) ...... 7.50 su-Ra
C43 -C44 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.351(8) ...... 7.50 su-Ra
C43 -N4 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.352(8) ...... 7.50 su-Ra
C44 -N2 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.7(6) ...... 5.00 su-Ra
N2 -C3 -N4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 114(3), Rep 113.2(5) ...... 6.00 su-Ra
N6 -C7 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(3), Rep 109.1(5) ...... 6.00 su-Ra
C10 -C9 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.2(5) ...... 6.00 su-Ra
C9 -C10 -N6 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.7(6) ...... 5.00 su-Ra
N11 -C12 -N13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C15 -C14 -N13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C14 -C15 -N11 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.8(6) ...... 5.00 su-Ra
N16 -C17 -N18 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.7(6) ...... 6.67 su-Ra
N20 -C21 -N22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 112(4), Rep 112.7(6) ...... 6.67 su-Ra
N24 -C25 -N26 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C28 -C27 -N26 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C27 -C28 -N24 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.8(6) ...... 5.00 su-Ra
N29 -C30 -N31 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C33 -C32 -N31 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(5) ...... 6.00 su-Ra
C32 -C33 -N29 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.8(6) ...... 5.00 su-Ra
N34 -C35 -N36 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.1(6) ...... 6.67 su-Ra
C38 -C37 -N36 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C37 -C38 -N34 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C40 -C39 -N22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C39 -C40 -N20 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C42 -C41 -N18 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C41 -C42 -N16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C44 -C43 -N4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C43 -C44 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 123(5), Rep 123.7(8) ...... 6.25 su-Ra
C112 -N1 -C111 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(6), Rep 110.1(8) ...... 7.50 su-Ra
C112 -N1 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 122(5), Rep 122.0(8) ...... 6.25 su-Ra
C111 -N1 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(5) ...... 6.00 su-Ra
C44 -N2 -C3 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(5) ...... 6.00 su-Ra
C43 -N4 -C3 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.3(5) ...... 6.00 su-Ra
C10 -N6 -C7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.3(5) ...... 6.00 su-Ra
C9 -N8 -C7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(5) ...... 6.00 su-Ra
C15 -N11 -C12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(5) ...... 6.00 su-Ra
C14 -N13 -C12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.5(5) ...... 6.00 su-Ra
C42 -N16 -C17 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(5) ...... 6.00 su-Ra
C41 -N18 -C17 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(5) ...... 8.00 su-Ra
C40 -N20 -C21 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(5) ...... 8.00 su-Ra
C39 -N22 -C21 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(5) ...... 6.00 su-Ra
C28 -N24 -C25 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(5) ...... 8.00 su-Ra
C27 -N26 -C25 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(5) ...... 6.00 su-Ra
C33 -N29 -C30 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(5) ...... 6.00 su-Ra
C32 -N31 -C30 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.5(5) ...... 6.00 su-Ra
C38 -N34 -C35 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.5(5) ...... 6.00 su-Ra
C37 -N36 -C35 1.555 1.555 1.555
722_ALERT_1_C Angle Calc 125.00, Rep 123.60 Dev... 1.40 Deg.
N26 -C25 -H251 1.555 1.555 1.555
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 is badly in error.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C111
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C112
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 12
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 17.735(9)
_cell_length_b 14.457(8)
_cell_length_c 14.829(9)
_cell_angle_alpha 90
_cell_angle_beta 100.25(5)
_cell_angle_gamma 90
_cell_volume 3741(4)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_int_tables_number 14
# 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 .
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
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 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 944.27
_cell_measurement_reflns_used 470
_cell_measurement_theta_min 3
_cell_measurement_theta_max 16
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.100
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_max 0.200
_exptl_crystal_density_diffrn 1.676
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.590
# Sheldrick geometric approximatio 0.60 0.77
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.52
_exptl_absorpt_correction_T_max 0.77
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_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 'USER DEFINED 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_reflns_number 1251
_reflns_number_total 1212
_diffrn_reflns_av_R_equivalents 0.000
# Number of reflections without Friedels Law is 1212
# Number of reflections with Friedels Law is 0
# Theoretical number of reflections is about 1732
_diffrn_reflns_theta_min 2.828
_diffrn_reflns_theta_max 15.709
_diffrn_measured_fraction_theta_max 0.701
_diffrn_reflns_theta_full 12.096
_diffrn_measured_fraction_theta_full 0.754
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -13
_reflns_limit_h_max 12
_reflns_limit_k_min 0
_reflns_limit_k_max 10
_reflns_limit_l_min 0
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 2.26
_oxford_diffrn_Wilson_scale 180.49
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.62
_refine_diff_density_max 0.67
# 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 602
_refine_ls_number_restraints 287
_refine_ls_number_parameters 237
_oxford_refine_ls_R_factor_ref 0.1369
_refine_ls_wR_factor_ref 0.1206
_refine_ls_goodness_of_fit_ref 1.2976
_refine_ls_shift/su_max 0.0056002
_refine_ls_shift/su_mean 0.0005411
# The values computed from all data
_oxford_reflns_number_all 1178
_refine_ls_R_factor_all 0.2125
_refine_ls_wR_factor_all 0.1415
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 602
_refine_ls_R_factor_gt 0.1369
_refine_ls_wR_factor_gt 0.1206
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.55 -0.465 1.00
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.4078(5) 0.1915(5) 0.1917(6) 0.0607 1.0000 Uani . U . . . . .
Zn5 Zn 0.2959(5) 0.5285(5) 0.3508(6) 0.0638 1.0000 Uani . U . . . . .
Zn19 Zn 0.0705(5) 0.7531(5) 0.1048(6) 0.0675 1.0000 Uani . U . . . . .
Zn23 Zn 0.1996(5) 1.0225(5) 0.3808(6) 0.0650 1.0000 Uani . U . . . . .
C1 C 0.163(4) 0.321(5) 0.181(6) 0.167(16) 1.0000 Uiso D U . . . . .
C3 C 0.3452(9) 0.361(3) 0.275(2) 0.071(11) 1.0000 Uiso D U . . . . .
C7 C 0.446(2) 0.623(2) 0.3213(15) 0.065(10) 1.0000 Uiso D U . . . . .
C9 C 0.466(2) 0.7349(18) 0.415(2) 0.065(10) 1.0000 Uiso D U . . . . .
C10 C 0.398(2) 0.695(3) 0.4228(17) 0.065(10) 1.0000 Uiso D U . . . . .
C11 C 0.367(4) 0.728(6) 0.117(7) 0.24(2) 1.0000 Uiso D U . . . . .
C12 C 0.3565(19) 0.409(2) 0.508(3) 0.082(10) 1.0000 Uiso D U . . . . .
C14 C 0.275(3) 0.399(2) 0.597(2) 0.082(10) 1.0000 Uiso D U . . . . .
C15 C 0.2461(18) 0.456(2) 0.526(3) 0.082(10) 1.0000 Uiso D U . . . . .
C17 C 0.186(2) 0.633(2) 0.235(3) 0.078(10) 1.0000 Uiso D U . . . . .
C21 C 0.1348(14) 0.899(3) 0.231(3) 0.069(10) 1.0000 Uiso D U . . . . .
C25 C 0.061(3) 1.148(3) 0.3879(14) 0.067(10) 1.0000 Uiso D U . . . . .
C27 C 0.104(4) 1.2680(19) 0.4647(18) 0.067(10) 1.0000 Uiso D U . . . . .
C28 C 0.163(2) 1.211(3) 0.4608(17) 0.067(10) 1.0000 Uiso D U . . . . .
C30 C 0.1214(18) 0.874(3) 0.4812(15) 0.066(11) 1.0000 Uiso D U . . . . .
C32 C 0.208(3) 0.770(2) 0.5101(15) 0.066(11) 1.0000 Uiso D U . . . . .
C33 C 0.2369(17) 0.843(4) 0.4698(16) 0.066(11) 1.0000 Uiso D U . . . . .
C35 C 0.315(2) 1.1228(19) 0.315(2) 0.059(9) 1.0000 Uiso D U . . . . .
C37 C 0.4296(18) 1.074(2) 0.359(3) 0.059(9) 1.0000 Uiso D U . . . . .
C38 C 0.383(3) 1.0297(16) 0.4078(16) 0.059(9) 1.0000 Uiso D U . . . . .
C39 C 0.1039(16) 1.031(2) 0.172(4) 0.069(10) 1.0000 Uiso D U . . . . .
C40 C 0.0800(11) 0.965(4) 0.108(2) 0.069(10) 1.0000 Uiso D U . . . . .
C41 C 0.0843(18) 0.655(2) 0.289(3) 0.078(10) 1.0000 Uiso D U . . . . .
C42 C 0.132(3) 0.600(2) 0.348(2) 0.078(10) 1.0000 Uiso D U . . . . .
C43 C 0.3323(9) 0.465(2) 0.172(3) 0.071(11) 1.0000 Uiso D U . . . . .
C44 C 0.3549(9) 0.386(4) 0.136(2) 0.071(11) 1.0000 Uiso D U . . . . .
C111 C 0.044(4) 0.370(5) 0.245(5) 0.167(16) 1.0000 Uiso D U . . . . .
C112 C 0.086(4) 0.445(5) 0.101(5) 0.166(16) 1.0000 Uiso D U . . . . .
C121 C 0.450(6) 0.870(5) 0.168(8) 0.24(2) 1.0000 Uiso D U . . . . .
C122 C 0.318(6) 0.836(7) 0.217(8) 0.24(2) 1.0000 Uiso D U . . . . .
N1 N 0.101(3) 0.386(3) 0.186(4) 0.166(16) 1.0000 Uiso D U . . . . .
N2 N 0.3632(7) 0.319(2) 0.201(3) 0.071(11) 1.0000 Uiso D U . . . . .
N4 N 0.3260(7) 0.450(3) 0.260(3) 0.070(11) 1.0000 Uiso D U . . . . .
N6 N 0.3852(18) 0.623(2) 0.363(2) 0.065(10) 1.0000 Uiso D U . . . . .
N8 N 0.4972(16) 0.690(3) 0.351(2) 0.065(10) 1.0000 Uiso D U . . . . .
N10 N 0.377(4) 0.820(4) 0.157(4) 0.24(2) 1.0000 Uiso D U . . . . .
N11 N 0.297(3) 0.4625(18) 0.469(2) 0.082(10) 1.0000 Uiso D U . . . . .
N13 N 0.345(2) 0.3692(16) 0.586(3) 0.082(10) 1.0000 Uiso D U . . . . .
N16 N 0.197(2) 0.5854(17) 0.314(3) 0.078(10) 1.0000 Uiso D U . . . . .
N18 N 0.118(3) 0.6760(16) 0.217(2) 0.078(10) 1.0000 Uiso D U . . . . .
N20 N 0.0994(17) 0.881(3) 0.145(4) 0.069(10) 1.0000 Uiso D U . . . . .
N22 N 0.1388(13) 0.990(4) 0.250(3) 0.069(10) 1.0000 Uiso D U . . . . .
N24 N 0.137(3) 1.134(2) 0.412(2) 0.067(10) 1.0000 Uiso D U . . . . .
N26 N 0.039(2) 1.229(3) 0.419(2) 0.067(10) 1.0000 Uiso D U . . . . .
N29 N 0.182(3) 0.909(2) 0.4510(11) 0.066(11) 1.0000 Uiso D U . . . . .
N31 N 0.135(2) 0.789(3) 0.5178(11) 0.066(11) 1.0000 Uiso D U . . . . .
N34 N 0.310(2) 1.060(2) 0.381(2) 0.059(9) 1.0000 Uiso D U . . . . .
N36 N 0.387(3) 1.1332(18) 0.2996(18) 0.059(9) 1.0000 Uiso D U . . . . .
O1 O 0.164(3) 0.252(4) 0.221(5) 0.167(16) 1.0000 Uiso D U . . . . .
O2 O 0.422(5) 0.684(4) 0.117(6) 0.24(2) 1.0000 Uiso D U . . . . .
H1221 H 0.3246 0.8972 0.2430 0.2854 1.0000 Uiso . . . . . . .
H1222 H 0.3238 0.7911 0.2646 0.2854 1.0000 Uiso . . . . . . .
H1223 H 0.2676 0.8315 0.1802 0.2854 1.0000 Uiso . . . . . . .
H1211 H 0.4787 0.8486 0.1226 0.2855 1.0000 Uiso . . . . . . .
H1212 H 0.4407 0.9353 0.1596 0.2855 1.0000 Uiso . . . . . . .
H1213 H 0.4793 0.8591 0.2279 0.2855 1.0000 Uiso . . . . . . .
H1111 H 0.0086 0.4205 0.2390 0.1996 1.0000 Uiso . . . . . . .
H1112 H 0.0700 0.3657 0.3077 0.1996 1.0000 Uiso . . . . . . .
H1113 H 0.0174 0.3134 0.2277 0.1996 1.0000 Uiso . . . . . . .
H1121 H 0.0454 0.4873 0.1051 0.1994 1.0000 Uiso . . . . . . .
H1122 H 0.1317 0.4783 0.0955 0.1994 1.0000 Uiso . . . . . . .
H1123 H 0.0718 0.4057 0.0483 0.1994 1.0000 Uiso . . . . . . .
H31 H 0.3459 0.3310 0.3307 0.0846 1.0000 Uiso . . . . . . .
H71 H 0.4527 0.5800 0.2763 0.0784 1.0000 Uiso . . . . . . .
H91 H 0.4879 0.7855 0.4491 0.0783 1.0000 Uiso . . . . . . .
H101 H 0.3662 0.7135 0.4624 0.0785 1.0000 Uiso . . . . . . .
H121 H 0.4006 0.4007 0.4827 0.0980 1.0000 Uiso . . . . . . .
H141 H 0.2503 0.3835 0.6451 0.0981 1.0000 Uiso . . . . . . .
H151 H 0.1986 0.4848 0.5179 0.0981 1.0000 Uiso . . . . . . .
H171 H 0.2222 0.6354 0.1962 0.0938 1.0000 Uiso . . . . . . .
H211 H 0.1543 0.8534 0.2727 0.0825 1.0000 Uiso . . . . . . .
H251 H 0.0284 1.1062 0.3534 0.0802 1.0000 Uiso . . . . . . .
H271 H 0.1067 1.3250 0.4942 0.0802 1.0000 Uiso . . . . . . .
H281 H 0.2142 1.2218 0.4872 0.0803 1.0000 Uiso . . . . . . .
H301 H 0.0749 0.9051 0.4771 0.0790 1.0000 Uiso . . . . . . .
H321 H 0.2341 0.7162 0.5295 0.0791 1.0000 Uiso . . . . . . .
H331 H 0.2864 0.8471 0.4573 0.0791 1.0000 Uiso . . . . . . .
H351 H 0.2737 1.1555 0.2837 0.0706 1.0000 Uiso . . . . . . .
H371 H 0.4822 1.0650 0.3649 0.0707 1.0000 Uiso . . . . . . .
H381 H 0.3984 0.9853 0.4528 0.0706 1.0000 Uiso . . . . . . .
H391 H 0.0974 1.0946 0.1630 0.0826 1.0000 Uiso . . . . . . .
H401 H 0.0545 0.9762 0.0485 0.0826 1.0000 Uiso . . . . . . .
H411 H 0.0361 0.6749 0.2976 0.0941 1.0000 Uiso . . . . . . .
H421 H 0.1217 0.5760 0.4027 0.0940 1.0000 Uiso . . . . . . .
H431 H 0.3227 0.5213 0.1410 0.0847 1.0000 Uiso . . . . . . .
H441 H 0.3636 0.3790 0.0761 0.0847 1.0000 Uiso . . . . . . .
H11 H 0.2004 0.3339 0.1459 0.1997 1.0000 Uiso . . . . . . .
H111 H 0.3189 0.7058 0.0918 0.2855 1.0000 Uiso . . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.074(6) 0.014(4) 0.096(8) 0.001(4) 0.020(6) 0.003(4)
Zn5 0.083(6) 0.019(4) 0.090(7) 0.002(4) 0.017(5) 0.010(5)
Zn19 0.089(7) 0.019(5) 0.092(7) -0.007(4) 0.007(5) 0.011(4)
Zn23 0.099(7) 0.014(4) 0.086(7) -0.005(4) 0.027(6) -0.001(5)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.0768(9)
loop_
_oxford_twin_element_scale_factors
0.701
0.299
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
Zn1 . N13 4_554 1.96(4) yes
Zn1 . N8 3_645 1.90(3) yes
Zn1 . N36 1_545 1.90(3) yes
Zn1 . N2 . 2.02(3) yes
Zn5 . N4 . 1.90(3) yes
Zn5 . N6 . 2.08(3) yes
Zn5 . N11 . 1.99(3) yes
Zn5 . N16 . 1.93(4) yes
Zn19 . N31 4_564 1.96(3) yes
Zn19 . N26 3_545 1.94(4) yes
Zn19 . N18 . 2.06(4) yes
Zn19 . N20 . 1.98(3) yes
Zn23 . N22 . 2.10(4) yes
Zn23 . N24 . 2.05(3) yes
Zn23 . N29 . 1.99(3) yes
Zn23 . N34 . 2.04(4) yes
C1 . N1 . 1.460(8) yes
C1 . O1 . 1.161(8) yes
C1 . H11 . 0.930 no
C3 . N2 . 1.345(8) yes
C3 . N4 . 1.344(8) yes
C3 . H31 . 0.930 no
C7 . N6 . 1.342(8) yes
C7 . N8 . 1.344(8) yes
C7 . H71 . 0.930 no
C9 . C10 . 1.357(8) yes
C9 . N8 . 1.352(8) yes
C9 . H91 . 0.930 no
C10 . N6 . 1.353(8) yes
C10 . H101 . 0.930 no
C11 . N10 . 1.459(8) yes
C11 . O2 . 1.159(8) yes
C11 . H111 . 0.930 no
C12 . N11 . 1.345(8) yes
C12 . N13 . 1.346(8) yes
C12 . H121 . 0.930 no
C14 . C15 . 1.356(8) yes
C14 . N13 . 1.352(8) yes
C14 . H141 . 0.930 no
C15 . N11 . 1.352(8) yes
C15 . H151 . 0.930 no
C17 . N16 . 1.344(8) yes
C17 . N18 . 1.345(8) yes
C17 . H171 . 0.930 no
C21 . N20 . 1.344(8) yes
C21 . N22 . 1.343(8) yes
C21 . H211 . 0.930 no
C25 . N24 . 1.346(8) yes
C25 . N26 . 1.346(8) yes
C25 . H251 . 0.930 no
C27 . C28 . 1.358(8) yes
C27 . N26 . 1.353(8) yes
C27 . H271 . 0.930 no
C28 . N24 . 1.354(8) yes
C28 . H281 . 0.930 no
C30 . N29 . 1.343(8) yes
C30 . N31 . 1.344(8) yes
C30 . H301 . 0.930 no
C32 . C33 . 1.357(8) yes
C32 . N31 . 1.352(8) yes
C32 . H321 . 0.930 no
C33 . N29 . 1.353(8) yes
C33 . H331 . 0.930 no
C35 . N34 . 1.345(8) yes
C35 . N36 . 1.345(8) yes
C35 . H351 . 0.930 no
C37 . C38 . 1.356(8) yes
C37 . N36 . 1.352(8) yes
C37 . H371 . 0.930 no
C38 . N34 . 1.353(8) yes
C38 . H381 . 0.930 no
C39 . C40 . 1.356(8) yes
C39 . N22 . 1.352(8) yes
C39 . H391 . 0.930 no
C40 . N20 . 1.352(8) yes
C40 . H401 . 0.930 no
C41 . C42 . 1.357(8) yes
C41 . N18 . 1.351(8) yes
C41 . H411 . 0.930 no
C42 . N16 . 1.352(8) yes
C42 . H421 . 0.930 no
C43 . C44 . 1.356(8) yes
C43 . N4 . 1.351(8) yes
C43 . H431 . 0.930 no
C44 . N2 . 1.352(8) yes
C44 . H441 . 0.930 no
C111 . N1 . 1.468(8) yes
C111 . H1111 . 0.960 no
C111 . H1112 . 0.960 no
C111 . H1113 . 0.961 no
C112 . N1 . 1.499(8) yes
C112 . H1121 . 0.960 no
C112 . H1122 . 0.960 no
C112 . H1123 . 0.960 no
C121 . N10 . 1.470(8) yes
C121 . H1211 . 0.959 no
C121 . H1212 . 0.960 no
C121 . H1213 . 0.960 no
C122 . N10 . 1.500(8) yes
C122 . H1221 . 0.960 no
C122 . H1222 . 0.960 no
C122 . H1223 . 0.961 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
N13 4_554 Zn1 . N8 3_645 98.0(17) yes
N13 4_554 Zn1 . N36 1_545 108.0(15) yes
N8 3_645 Zn1 . N36 1_545 126(2) yes
N13 4_554 Zn1 . N2 . 106.7(11) yes
N8 3_645 Zn1 . N2 . 114.5(16) yes
N36 1_545 Zn1 . N2 . 102.5(18) yes
N4 . Zn5 . N6 . 98.6(16) yes
N4 . Zn5 . N11 . 112.0(20) yes
N6 . Zn5 . N11 . 110.3(11) yes
N4 . Zn5 . N16 . 114.2(14) yes
N6 . Zn5 . N16 . 112.7(11) yes
N11 . Zn5 . N16 . 109(2) yes
N31 4_564 Zn19 . N26 3_545 120.2(14) yes
N31 4_564 Zn19 . N18 . 99.3(16) yes
N26 3_545 Zn19 . N18 . 108(2) yes
N31 4_564 Zn19 . N20 . 109.8(16) yes
N26 3_545 Zn19 . N20 . 114.7(16) yes
N18 . Zn19 . N20 . 102.6(19) yes
N22 . Zn23 . N24 . 100.3(18) yes
N22 . Zn23 . N29 . 101.4(16) yes
N24 . Zn23 . N29 . 112.9(14) yes
N22 . Zn23 . N34 . 113.2(9) yes
N24 . Zn23 . N34 . 110.3(17) yes
N29 . Zn23 . N34 . 117(2) yes
N1 . C1 . O1 . 118.1(8) yes
N1 . C1 . H11 . 120.9 no
O1 . C1 . H11 . 121.0 no
N2 . C3 . N4 . 112.7(6) yes
N2 . C3 . H31 . 123.7 no
N4 . C3 . H31 . 123.7 no
N6 . C7 . N8 . 113.2(5) yes
N6 . C7 . H71 . 123.4 no
N8 . C7 . H71 . 123.4 no
C10 . C9 . N8 . 109.1(5) yes
C10 . C9 . H91 . 125.5 no
N8 . C9 . H91 . 125.5 no
C9 . C10 . N6 . 109.2(5) yes
C9 . C10 . H101 . 125.4 no
N6 . C10 . H101 . 125.4 no
N10 . C11 . O2 . 117.9(8) yes
N10 . C11 . H111 . 121.1 no
O2 . C11 . H111 . 121.0 no
N11 . C12 . N13 . 112.7(6) yes
N11 . C12 . H121 . 123.6 no
N13 . C12 . H121 . 123.7 no
C15 . C14 . N13 . 109.1(6) yes
C15 . C14 . H141 . 125.5 no
N13 . C14 . H141 . 125.4 no
C14 . C15 . N11 . 109.1(6) yes
C14 . C15 . H151 . 125.4 no
N11 . C15 . H151 . 125.5 no
N16 . C17 . N18 . 112.8(6) yes
N16 . C17 . H171 . 123.7 no
N18 . C17 . H171 . 123.5 no
N20 . C21 . N22 . 112.7(6) yes
N20 . C21 . H211 . 123.6 no
N22 . C21 . H211 . 123.7 no
N24 . C25 . N26 . 112.7(6) yes
N24 . C25 . H251 . 123.6 no
N26 . C25 . H251 . 123.6 no
C28 . C27 . N26 . 109.1(6) yes
C28 . C27 . H271 . 125.5 no
N26 . C27 . H271 . 125.4 no
C27 . C28 . N24 . 109.0(6) yes
C27 . C28 . H281 . 125.5 no
N24 . C28 . H281 . 125.5 no
N29 . C30 . N31 . 112.8(6) yes
N29 . C30 . H301 . 123.6 no
N31 . C30 . H301 . 123.6 no
C33 . C32 . N31 . 109.0(6) yes
C33 . C32 . H321 . 125.5 no
N31 . C32 . H321 . 125.5 no
C32 . C33 . N29 . 109.0(5) yes
C32 . C33 . H331 . 125.5 no
N29 . C33 . H331 . 125.5 no
N34 . C35 . N36 . 112.8(6) yes
N34 . C35 . H351 . 123.6 no
N36 . C35 . H351 . 123.6 no
C38 . C37 . N36 . 109.1(6) yes
C38 . C37 . H371 . 125.4 no
N36 . C37 . H371 . 125.5 no
C37 . C38 . N34 . 109.1(6) yes
C37 . C38 . H381 . 125.5 no
N34 . C38 . H381 . 125.4 no
C40 . C39 . N22 . 109.0(6) yes
C40 . C39 . H391 . 125.5 no
N22 . C39 . H391 . 125.5 no
C39 . C40 . N20 . 109.0(6) yes
C39 . C40 . H401 . 125.5 no
N20 . C40 . H401 . 125.5 no
C42 . C41 . N18 . 109.0(6) yes
C42 . C41 . H411 . 125.5 no
N18 . C41 . H411 . 125.6 no
C41 . C42 . N16 . 109.1(6) yes
C41 . C42 . H421 . 125.5 no
N16 . C42 . H421 . 125.4 no
C44 . C43 . N4 . 109.1(6) yes
C44 . C43 . H431 . 125.4 no
N4 . C43 . H431 . 125.5 no
C43 . C44 . N2 . 109.0(6) yes
C43 . C44 . H441 . 125.5 no
N2 . C44 . H441 . 125.5 no
N1 . C111 . H1111 . 109.5 no
N1 . C111 . H1112 . 109.5 no
H1111 . C111 . H1112 . 109.5 no
N1 . C111 . H1113 . 109.5 no
H1111 . C111 . H1113 . 109.4 no
H1112 . C111 . H1113 . 109.5 no
N1 . C112 . H1121 . 109.5 no
N1 . C112 . H1122 . 109.5 no
H1121 . C112 . H1122 . 109.4 no
N1 . C112 . H1123 . 109.5 no
H1121 . C112 . H1123 . 109.5 no
H1122 . C112 . H1123 . 109.5 no
N10 . C121 . H1211 . 109.4 no
N10 . C121 . H1212 . 109.4 no
H1211 . C121 . H1212 . 109.5 no
N10 . C121 . H1213 . 109.4 no
H1211 . C121 . H1213 . 109.5 no
H1212 . C121 . H1213 . 109.5 no
N10 . C122 . H1221 . 109.5 no
N10 . C122 . H1222 . 109.6 no
H1221 . C122 . H1222 . 109.5 no
N10 . C122 . H1223 . 109.5 no
H1221 . C122 . H1223 . 109.4 no
H1222 . C122 . H1223 . 109.4 no
C112 . N1 . C111 . 123.7(8) yes
C112 . N1 . C1 . 110.1(8) yes
C111 . N1 . C1 . 122.0(8) yes
C44 . N2 . C3 . 104.6(5) yes
C44 . N2 . Zn1 . 127(3) yes
C3 . N2 . Zn1 . 128(3) yes
C43 . N4 . C3 . 104.6(5) yes
C43 . N4 . Zn5 . 132(4) yes
C3 . N4 . Zn5 . 123(4) yes
C10 . N6 . C7 . 104.3(5) yes
C10 . N6 . Zn5 . 127(3) yes
C7 . N6 . Zn5 . 128(3) yes
C9 . N8 . C7 . 104.3(5) yes
C9 . N8 . Zn1 3_655 136(3) yes
C7 . N8 . Zn1 3_655 119(3) yes
C122 . N10 . C121 . 124.0(8) yes
C122 . N10 . C11 . 109.8(8) yes
C121 . N10 . C11 . 121.9(8) yes
C15 . N11 . C12 . 104.6(5) yes
C15 . N11 . Zn5 . 133(4) yes
C12 . N11 . Zn5 . 123(4) yes
C14 . N13 . C12 . 104.6(5) yes
C14 . N13 . Zn1 4_555 117(4) yes
C12 . N13 . Zn1 4_555 137(4) yes
C42 . N16 . C17 . 104.5(5) yes
C42 . N16 . Zn5 . 139(3) yes
C17 . N16 . Zn5 . 116(3) yes
C41 . N18 . C17 . 104.6(5) yes
C41 . N18 . Zn19 . 126(3) yes
C17 . N18 . Zn19 . 129(3) yes
C40 . N20 . C21 . 104.6(5) yes
C40 . N20 . Zn19 . 133(4) yes
C21 . N20 . Zn19 . 121(4) yes
C39 . N22 . C21 . 104.6(5) yes
C39 . N22 . Zn23 . 141(4) yes
C21 . N22 . Zn23 . 114(4) yes
C28 . N24 . C25 . 104.6(5) yes
C28 . N24 . Zn23 . 128(4) yes
C25 . N24 . Zn23 . 127(4) yes
C27 . N26 . C25 . 104.6(5) yes
C27 . N26 . Zn19 3_555 139(4) yes
C25 . N26 . Zn19 3_555 117(4) yes
C33 . N29 . C30 . 104.6(5) yes
C33 . N29 . Zn23 . 121(3) yes
C30 . N29 . Zn23 . 134(3) yes
C32 . N31 . C30 . 104.6(5) yes
C32 . N31 . Zn19 4_565 132(3) yes
C30 . N31 . Zn19 4_565 118(3) yes
C38 . N34 . C35 . 104.5(5) yes
C38 . N34 . Zn23 . 141(3) yes
C35 . N34 . Zn23 . 112(3) yes
C37 . N36 . C35 . 104.5(5) yes
C37 . N36 . Zn1 1_565 131(3) yes
C35 . N36 . Zn1 1_565 121(3) yes
# Attachment '- phaseII_99.cif'
data_phaseII_99
_database_code_depnum_ccdc_archive 'CCDC 828172'
#TrackingRef '- phaseII_99.cif'
_audit_creation_date 11-03-21
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title 'phase2 in P2(1)/c'
_chemical_name_systematic ?
_chemical_name_common ZIF-4
_chemical_formula_moiety 'C24 H24 N16 Zn4, 2(C3 H7 N O)'
# Given Formula = C38 H40 N10 O2 Zn4
# Dc = 1.69 Fooo = 1920.00 Mu = 26.38 M = 930.32
# Found Formula = C30 H38 N18 O2 Zn4
# Dc = 1.71 FOOO = 1920.00 Mu = 26.45 M = 944.27
_chemical_formula_sum 'C30 H38 N18 O2 Zn4'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure 990
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.41
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6].. 16.89 Deg.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 14.52 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.52
088_ALERT_3_A Poor Data / Parameter Ratio .................... 3.98
201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 40
341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 54
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.422 1326
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 6
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 230
All of the above are caused by shading from the pressure cell. 1,2 and 1,3
restraints were applied to all non-hydrogen distances.
220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.69 Ratio
220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.69 Ratio
This is caused by DMF solvent in the pores.
082_ALERT_2_C High R1 Value .................................. 0.13
084_ALERT_2_C High R2 Value .................................. 0.31
153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 500 Ang.
The sample has undergone a phase transition which caused the crystal to
'break up', increasing the R1 value and increasing e.s.d's on measured
unit cell dimensions.
411_ALERT_2_C Short Inter H...H Contact H1031 .. H201 .. 2.06 Ang.
432_ALERT_2_C Short Inter X...Y Contact O2 .. C3 .. 3.00 Ang.
432_ALERT_2_C Short Inter X...Y Contact C7 .. C201 .. 3.12 Ang.
411_ALERT_2_A Short Inter H...H Contact H1031 .. H51 .. 1.75 Ang.
411_ALERT_2_B Short Inter H...H Contact H1031 .. H61 .. 1.87 Ang.
413_ALERT_2_B Short Inter XH3 .. XHn H2023 .. H151 .. 2.09 Ang.
432_ALERT_2_B Short Inter X...Y Contact C5 .. C103 .. 2.99 Ang.
432_ALERT_2_B Short Inter X...Y Contact C6 .. C103 .. 3.04 Ang.
432_ALERT_2_B Short Inter X...Y Contact C22 .. C104 .. 3.05 Ang.
Short contacts are expected at high-pressure.
344_ALERT_2_G Check sp? Angle Range in Solvent/Ion for .... C103
This is correct.
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.349(8) ...... 8.75 su-Ra
C6 -N4 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(7), Rep 1.343(8) ...... 8.75 su-Ra
C10 -N7 1.555 1.555
731_ALERT_1_A Bond Calc 1.35(8), Rep 1.343(8) ...... 9.90 su-Ra
C10 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.36(7), Rep 1.351(8) ...... 8.75 su-Ra
C11 -N8 1.555 1.555
731_ALERT_1_A Bond Calc 1.50(12), Rep 1.500(9) ...... 9.90 su-Ra
C101 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.47(11), Rep 1.471(9) ...... 9.90 su-Ra
C102 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(10), Rep 1.460(9) ...... 9.90 su-Ra
C103 -N17 1.555 1.555
731_ALERT_1_A Bond Calc 1.16(11), Rep 1.158(9) ...... 9.90 su-Ra
C103 -O2 1.555 1.555
731_ALERT_1_A Bond Calc 1.45(9), Rep 1.458(9) ...... 9.90 su-Ra
C104 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.17(10), Rep 1.160(9) ...... 9.90 su-Ra
C104 -O1 1.555 1.555
731_ALERT_1_A Bond Calc 1.50(9), Rep 1.497(9) ...... 9.90 su-Ra
C201 -N18 1.555 1.555
731_ALERT_1_A Bond Calc 1.46(9), Rep 1.468(9) ...... 9.90 su-Ra
C202 -N18 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(4), Rep 1.344(8) ...... 5.00 su-Ra
C1 -N1 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.347(8) ...... 6.25 su-Ra
C1 -N2 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(4), Rep 1.356(8) ...... 5.00 su-Ra
C2 -C3 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.355(8) ...... 6.25 su-Ra
C2 -N1 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(4), Rep 1.350(8) ...... 5.00 su-Ra
C3 -N2 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.342(8) ...... 7.50 su-Ra
C4 -N3 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.343(8) ...... 7.50 su-Ra
C4 -N4 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.356(8) ...... 7.50 su-Ra
C5 -C6 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.353(8) ...... 7.50 su-Ra
C5 -N3 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(5), Rep 1.345(8) ...... 6.25 su-Ra
C7 -N5 1.555 1.555
731_ALERT_1_B Bond Calc 1.33(5), Rep 1.346(8) ...... 6.25 su-Ra
C7 -N6 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.360(8) ...... 7.50 su-Ra
C8 -C9 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.352(8) ...... 7.50 su-Ra
C8 -N6 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.354(8) ...... 6.25 su-Ra
C9 -N5 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.356(8) ...... 7.50 su-Ra
C11 -C12 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(7), Rep 1.355(9) ...... 7.78 su-Ra
C12 -N7 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.344(8) ...... 7.50 su-Ra
C13 -N9 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.344(8) ...... 7.50 su-Ra
C13 -N10 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.358(8) ...... 6.25 su-Ra
C14 -C15 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.351(8) ...... 7.50 su-Ra
C14 -N10 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.349(8) ...... 7.50 su-Ra
C15 -N9 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.346(8) ...... 7.50 su-Ra
C16 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.343(8) ...... 7.50 su-Ra
C16 -N12 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.356(8) ...... 6.25 su-Ra
C17 -C18 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.356(8) ...... 7.50 su-Ra
C17 -N12 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.352(8) ...... 7.50 su-Ra
C18 -N11 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.341(8) ...... 7.50 su-Ra
C19 -N13 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.345(8) ...... 7.50 su-Ra
C19 -N14 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.358(8) ...... 7.50 su-Ra
C20 -C21 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.354(8) ...... 7.50 su-Ra
C20 -N13 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(6), Rep 1.350(8) ...... 7.50 su-Ra
C21 -N14 1.555 1.555
731_ALERT_1_B Bond Calc 1.34(6), Rep 1.346(8) ...... 7.50 su-Ra
C22 -N15 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.346(8) ...... 6.25 su-Ra
C22 -N16 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.357(8) ...... 6.25 su-Ra
C23 -C24 1.555 1.555
731_ALERT_1_B Bond Calc 1.36(6), Rep 1.351(8) ...... 7.50 su-Ra
C23 -N15 1.555 1.555
731_ALERT_1_B Bond Calc 1.35(5), Rep 1.354(8) ...... 6.25 su-Ra
C24 -N16 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.8(6) ...... 5.00 su-Ra
N1 -C1 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C2 -C3 -N2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 112.8(6) ...... 6.67 su-Ra
N3 -C4 -N4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 109.0(6) ...... 6.67 su-Ra
C6 -C5 -N3 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(3), Rep 109.0(6) ...... 5.00 su-Ra
C5 -C6 -N4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.9(6) ...... 5.00 su-Ra
N5 -C7 -N6 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C9 -C8 -N6 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C8 -C9 -N5 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 113.0(7) ...... 5.71 su-Ra
N7 -C10 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(4), Rep 108.9(7) ...... 5.71 su-Ra
C12 -C11 -N8 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(4), Rep 109.2(6) ...... 6.67 su-Ra
C11 -C12 -N7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.9(6) ...... 5.00 su-Ra
N9 -C13 -N10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(3), Rep 109.1(6) ...... 5.00 su-Ra
C15 -C14 -N10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C14 -C15 -N9 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.7(6) ...... 5.00 su-Ra
N11 -C16 -N12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(4), Rep 109.0(6) ...... 6.67 su-Ra
C18 -C17 -N12 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C17 -C18 -N11 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(4), Rep 113.3(6) ...... 6.67 su-Ra
N13 -C19 -N14 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.3(6) ...... 5.00 su-Ra
C21 -C20 -N13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C20 -C21 -N14 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 113(3), Rep 112.7(6) ...... 5.00 su-Ra
N15 -C22 -N16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.1(6) ...... 5.00 su-Ra
C24 -C23 -N15 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 109(3), Rep 109.0(6) ...... 5.00 su-Ra
C23 -C24 -N16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 119(7), Rep 118.1(9) ...... 7.78 su-Ra
N17 -C103 -O2 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.4(6) ...... 5.00 su-Ra
C2 -N1 -C1 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.5(6) ...... 5.00 su-Ra
C5 -N3 -C4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.7(6) ...... 6.67 su-Ra
C6 -N4 -C4 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.5(6) ...... 5.00 su-Ra
C9 -N5 -C7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.5(6) ...... 5.00 su-Ra
C8 -N6 -C7 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.3(6) ...... 6.67 su-Ra
C12 -N7 -C10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(4), Rep 104.6(8) ...... 5.00 su-Ra
C11 -N8 -C10 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 105(3), Rep 104.6(6) ...... 5.00 su-Ra
C15 -N9 -C13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.4(6) ...... 5.00 su-Ra
C14 -N10 -C13 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.7(6) ...... 5.00 su-Ra
C18 -N11 -C16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(6) ...... 5.00 su-Ra
C17 -N12 -C16 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.1(6) ...... 5.00 su-Ra
C20 -N13 -C19 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(4), Rep 104.4(6) ...... 6.67 su-Ra
C21 -N14 -C19 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.6(6) ...... 5.00 su-Ra
C23 -N15 -C22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 104(3), Rep 104.5(6) ...... 5.00 su-Ra
C24 -N16 -C22 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 124(7), Rep 124.1(9) ...... 7.78 su-Ra
C101 -N17 -C102 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(6), Rep 109.9(9) ...... 6.67 su-Ra
C101 -N17 -C103 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 122(6), Rep 122.0(9) ...... 6.67 su-Ra
C102 -N17 -C103 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 124(5), Rep 123.5(9) ...... 5.56 su-Ra
C201 -N18 -C202 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 110(5), Rep 110.2(9) ...... 5.56 su-Ra
C201 -N18 -C104 1.555 1.555 1.555
732_ALERT_1_B Angle Calc 122(5), Rep 122.0(9) ...... 5.56 su-Ra
C202 -N18 -C104 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 109(2), Rep 109.2(6) ...... 3.33 su-Ra
C3 -C2 -N1 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 105(2), Rep 104.6(6) ...... 3.33 su-Ra
C3 -N2 -C1 1.555 1.555 1.555
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 is badly in error.
092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka .. 0.69 Ang.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 14
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 17.608(5)
_cell_length_b 14.411(5)
_cell_length_c 14.703(5)
_cell_angle_alpha 90
_cell_angle_beta 100.90(2)
_cell_angle_gamma 90
_cell_volume 3663.3(19)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_int_tables_number 14
# 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 .
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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 0.0029 0.0015 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 0.0057 0.0031 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 0.0101 0.0057 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'
Zn 0.3006 1.3591 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
_chemical_formula_weight 944.27
_cell_measurement_reflns_used 1044
_cell_measurement_theta_min 2
_cell_measurement_theta_max 17
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.140
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_max 0.220
_exptl_crystal_density_diffrn 1.712
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.645
# Sheldrick geometric approximatio 0.64 0.69
_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 0.69
_diffrn_measurement_device_type Unknown
_diffrn_measurement_device Serial
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.68890
_diffrn_source synchrotron
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'USER DEFINED DATA COLLECTION'
_computing_cell_refinement 'USER DEFINED CELL REFINEMENT'
_computing_data_reduction 'USER DEFINED DATA REDUCTION'
_computing_structure_solution 'USER DEFINED 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_reflns_number 1857
_reflns_number_total 948
_diffrn_reflns_av_R_equivalents 0.077
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 948
# Theoretical number of reflections is about 4604
_diffrn_reflns_theta_min 1.783
_diffrn_reflns_theta_max 16.890
_diffrn_measured_fraction_theta_max 0.411
_diffrn_reflns_theta_full 14.525
_diffrn_measured_fraction_theta_full 0.519
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 11
_reflns_limit_h_min -14
_reflns_limit_h_max 13
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 11
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.74
_refine_diff_density_max 0.71
# 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>-10.0\s(I)
_refine_ls_number_reflns 948
_refine_ls_number_restraints 230
_refine_ls_number_parameters 238
_oxford_refine_ls_R_factor_ref 0.1609
_refine_ls_wR_factor_ref 0.3074
_refine_ls_goodness_of_fit_ref 1.0741
_refine_ls_shift/su_max 0.0300659
_refine_ls_shift/su_mean 0.0020829
# The values computed from all data
_oxford_reflns_number_all 948
_refine_ls_R_factor_all 0.1609
_refine_ls_wR_factor_all 0.3074
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 684
_refine_ls_R_factor_gt 0.1336
_refine_ls_wR_factor_gt 0.2972
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
17.3 18.1 5.98
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
User-defined data collection reference
User defined data reduction
User defined cell refinement
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.2000(5) 1.0256(6) 0.3854(6) 0.0635 1.0000 Uani . . . . . . .
Zn2 Zn 0.0690(5) 0.7434(6) 0.6028(6) 0.0627 1.0000 Uani . . . . . . .
Zn3 Zn 0.2948(5) 0.9691(6) 0.8514(6) 0.0600 1.0000 Uani . . . . . . .
Zn4 Zn 0.4090(5) 1.1922(6) 0.1936(6) 0.0649 1.0000 Uani . . . . . . .
C1 C 0.3174(18) 1.1212(17) 0.3209(16) 0.036(8) 1.0000 Uiso D U . . . . .
C2 C 0.383(2) 1.0236(14) 0.4128(14) 0.036(8) 1.0000 Uiso D U . . . . .
C3 C 0.4318(16) 1.069(2) 0.367(2) 0.036(8) 1.0000 Uiso D U . . . . .
C4 C 0.123(2) 0.881(3) 0.4812(15) 0.076(11) 1.0000 Uiso D U . . . . .
C5 C 0.2400(19) 0.843(4) 0.4792(16) 0.076(11) 1.0000 Uiso D U . . . . .
C6 C 0.205(3) 0.772(2) 0.5157(13) 0.076(11) 1.0000 Uiso D U . . . . .
C7 C 0.064(2) 1.147(2) 0.4011(11) 0.046(9) 1.0000 Uiso D U . . . . .
C8 C 0.108(3) 1.2739(18) 0.4645(12) 0.046(9) 1.0000 Uiso D U . . . . .
C9 C 0.1685(18) 1.218(3) 0.4584(13) 0.046(9) 1.0000 Uiso D U . . . . .
C10 C 0.1410(15) 0.896(3) 0.237(4) 0.068(10) 1.0000 Uiso D U . . . . .
C11 C 0.0834(11) 0.964(4) 0.114(2) 0.069(10) 1.0000 Uiso D U . . . . .
C12 C 0.1084(16) 1.029(2) 0.179(4) 0.069(10) 1.0000 Uiso D U . . . . .
C13 C 0.183(2) 0.867(2) 0.733(3) 0.076(10) 1.0000 Uiso D U . . . . .
C14 C 0.130(3) 0.8994(19) 0.848(2) 0.076(10) 1.0000 Uiso D U . . . . .
C15 C 0.0808(18) 0.845(2) 0.789(3) 0.076(10) 1.0000 Uiso D U . . . . .
C16 C 0.358(2) 1.083(2) 0.014(3) 0.072(10) 1.0000 Uiso D U . . . . .
C17 C 0.274(3) 1.103(2) 0.099(2) 0.072(10) 1.0000 Uiso D U . . . . .
C18 C 0.2431(18) 1.0469(19) 0.028(3) 0.072(10) 1.0000 Uiso D U . . . . .
C19 C 0.553(3) 1.122(3) 0.1824(19) 0.097(12) 1.0000 Uiso D U . . . . .
C20 C 0.598(2) 1.196(3) 0.079(2) 0.097(12) 1.0000 Uiso D U . . . . .
C21 C 0.532(3) 1.238(2) 0.092(3) 0.097(12) 1.0000 Uiso D U . . . . .
C22 C 0.3396(10) 1.364(3) 0.271(2) 0.069(10) 1.0000 Uiso D U . . . . .
C23 C 0.3292(10) 1.468(2) 0.167(3) 0.069(10) 1.0000 Uiso D U . . . . .
C24 C 0.3545(10) 1.389(3) 0.133(2) 0.069(10) 1.0000 Uiso D U . . . . .
C101 C 0.327(5) 0.655(7) 0.718(7) 0.23(3) 1.0000 Uiso D U . . . . .
C102 C 0.456(5) 0.622(5) 0.659(7) 0.23(3) 1.0000 Uiso D U . . . . .
C103 C 0.372(4) 0.767(5) 0.617(7) 0.23(3) 1.0000 Uiso D U . . . . .
C104 C 0.168(4) 1.331(5) 0.197(6) 0.164(18) 1.0000 Uiso D U . . . . .
C201 C 0.086(4) 1.440(6) 0.099(5) 0.164(18) 1.0000 Uiso D U . . . . .
C202 C 0.038(4) 1.368(6) 0.241(6) 0.164(18) 1.0000 Uiso D U . . . . .
N1 N 0.3101(18) 1.0559(19) 0.3840(18) 0.036(8) 1.0000 Uiso D U . . . . .
N2 N 0.391(2) 1.1316(16) 0.3089(15) 0.036(8) 1.0000 Uiso D U . . . . .
N3 N 0.188(3) 0.913(2) 0.4572(11) 0.076(11) 1.0000 Uiso D U . . . . .
N4 N 0.131(3) 0.795(3) 0.5173(13) 0.076(11) 1.0000 Uiso D U . . . . .
N5 N 0.142(2) 1.137(2) 0.4185(14) 0.046(9) 1.0000 Uiso D U . . . . .
N6 N 0.0411(18) 1.229(3) 0.4283(15) 0.046(9) 1.0000 Uiso D U . . . . .
N7 N 0.1454(13) 0.987(4) 0.258(3) 0.068(10) 1.0000 Uiso D U . . . . .
N8 N 0.1037(19) 0.879(3) 0.150(4) 0.068(10) 1.0000 Uiso D U . . . . .
N9 N 0.114(3) 0.8245(16) 0.715(2) 0.076(10) 1.0000 Uiso D U . . . . .
N10 N 0.195(2) 0.9143(16) 0.814(3) 0.076(10) 1.0000 Uiso D U . . . . .
N11 N 0.296(3) 1.0339(17) -0.0271(19) 0.072(10) 1.0000 Uiso D U . . . . .
N12 N 0.347(2) 1.1267(16) 0.091(3) 0.072(10) 1.0000 Uiso D U . . . . .
N13 N 0.612(2) 1.122(3) 0.136(3) 0.097(12) 1.0000 Uiso D U . . . . .
N14 N 0.5030(18) 1.192(3) 0.158(3) 0.096(12) 1.0000 Uiso D U . . . . .
N15 N 0.3194(8) 1.453(3) 0.255(3) 0.069(10) 1.0000 Uiso D U . . . . .
N16 N 0.3612(8) 1.322(2) 0.198(3) 0.069(10) 1.0000 Uiso D U . . . . .
N17 N 0.383(4) 0.673(4) 0.655(4) 0.23(3) 1.0000 Uiso D U . . . . .
N18 N 0.099(3) 1.388(3) 0.189(3) 0.164(18) 1.0000 Uiso D U . . . . .
O1 O 0.164(4) 1.259(4) 0.232(5) 0.164(18) 1.0000 Uiso D U . . . . .
O2 O 0.426(5) 0.813(4) 0.617(6) 0.23(3) 1.0000 Uiso D U . . . . .
H11 H 0.2750 1.1569 0.2899 0.0384 1.0000 Uiso R . . . . . .
H21 H 0.3980 0.9754 0.4565 0.0384 1.0000 Uiso R . . . . . .
H31 H 0.4859 1.0594 0.3739 0.0385 1.0000 Uiso R . . . . . .
H41 H 0.0771 0.9165 0.4702 0.1104 1.0000 Uiso R . . . . . .
H51 H 0.2926 0.8415 0.4727 0.1104 1.0000 Uiso R . . . . . .
H61 H 0.2278 0.7150 0.5403 0.1104 1.0000 Uiso R . . . . . .
H71 H 0.0297 1.1017 0.3688 0.0639 1.0000 Uiso R . . . . . .
H81 H 0.1109 1.3333 0.4931 0.0638 1.0000 Uiso R . . . . . .
H91 H 0.2213 1.2318 0.4820 0.0639 1.0000 Uiso R . . . . . .
H101 H 0.1627 0.8499 0.2801 0.0882 1.0000 Uiso R . . . . . .
H111 H 0.0555 0.9743 0.0530 0.0884 1.0000 Uiso R . . . . . .
H121 H 0.1006 1.0940 0.1698 0.0883 1.0000 Uiso R . . . . . .
H131 H 0.2189 0.8663 0.6928 0.0942 1.0000 Uiso R . . . . . .
H141 H 0.1202 0.9223 0.9055 0.0944 1.0000 Uiso R . . . . . .
H151 H 0.0316 0.8236 0.7971 0.0945 1.0000 Uiso R . . . . . .
H161 H 0.4041 1.0867 -0.0108 0.0988 1.0000 Uiso R . . . . . .
H171 H 0.2491 1.1236 0.1476 0.0989 1.0000 Uiso R . . . . . .
H181 H 0.1927 1.0210 0.0189 0.0989 1.0000 Uiso R . . . . . .
H191 H 0.5462 1.0779 0.2283 0.1058 1.0000 Uiso R . . . . . .
H201 H 0.6305 1.2138 0.0374 0.1059 1.0000 Uiso R . . . . . .
H211 H 0.5111 1.2921 0.0593 0.1058 1.0000 Uiso R . . . . . .
H221 H 0.3383 1.3341 0.3287 0.0925 1.0000 Uiso R . . . . . .
H231 H 0.3199 1.5250 0.1336 0.0925 1.0000 Uiso R . . . . . .
H241 H 0.3660 1.3809 0.0726 0.0926 1.0000 Uiso R . . . . . .
H1011 H 0.2812 0.6912 0.6961 0.2979 1.0000 Uiso R . . . . . .
H1012 H 0.3528 0.6786 0.7766 0.2979 1.0000 Uiso R . . . . . .
H1013 H 0.3127 0.5915 0.7244 0.2979 1.0000 Uiso R . . . . . .
H1021 H 0.4795 0.6365 0.6064 0.2979 1.0000 Uiso R . . . . . .
H1022 H 0.4887 0.6438 0.7143 0.2979 1.0000 Uiso R . . . . . .
H1023 H 0.4487 0.5566 0.6621 0.2979 1.0000 Uiso R . . . . . .
H2011 H 0.0388 1.4753 0.0890 0.2346 1.0000 Uiso R . . . . . .
H2012 H 0.1292 1.4818 0.1037 0.2346 1.0000 Uiso R . . . . . .
H2013 H 0.0857 1.3989 0.0474 0.2346 1.0000 Uiso R . . . . . .
H2021 H -0.0032 1.4118 0.2216 0.2346 1.0000 Uiso R . . . . . .
H2022 H 0.0533 1.3696 0.3068 0.2346 1.0000 Uiso R . . . . . .
H2023 H 0.0204 1.3069 0.2212 0.2346 1.0000 Uiso R . . . . . .
H1041 H 0.2152 1.3610 0.1839 0.2347 1.0000 Uiso R . . . . . .
H1031 H 0.3249 0.7711 0.5695 0.2980 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.078(8) 0.052(8) 0.059(9) 0.002(5) 0.010(7) 0.002(5)
Zn2 0.079(8) 0.039(8) 0.071(9) 0.016(5) 0.014(7) 0.003(5)
Zn3 0.061(7) 0.056(8) 0.064(9) 0.002(5) 0.015(7) 0.007(5)
Zn4 0.072(8) 0.060(8) 0.066(9) -0.001(5) 0.021(7) -0.026(5)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.1229(3)
loop_
_oxford_twin_element_scale_factors
0.756(13)
0.244(13)
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
Zn1 . N1 . 1.99(3) yes
Zn1 . N3 . 1.97(3) yes
Zn1 . N5 . 2.01(3) yes
Zn1 . N7 . 2.02(4) yes
Zn2 . N8 4_565 1.95(3) yes
Zn2 . N6 2_576 1.95(3) yes
Zn2 . N4 . 1.96(3) yes
Zn2 . N9 . 2.06(4) yes
Zn3 . N13 2_676 2.08(4) yes
Zn3 . N11 1_556 2.01(3) yes
Zn3 . N15 4_575 1.92(3) yes
Zn3 . N10 . 1.92(4) yes
Zn4 . N2 . 1.99(3) yes
Zn4 . N12 . 1.94(4) yes
Zn4 . N14 . 1.83(4) yes
Zn4 . N16 . 2.06(3) yes
C1 . N1 . 1.344(8) yes
C1 . N2 . 1.347(8) yes
C1 . H11 . 0.950 no
C2 . C3 . 1.356(8) yes
C2 . N1 . 1.355(8) yes
C2 . H21 . 0.950 no
C3 . N2 . 1.350(8) yes
C3 . H31 . 0.950 no
C4 . N3 . 1.342(8) yes
C4 . N4 . 1.343(8) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.356(8) yes
C5 . N3 . 1.353(8) yes
C5 . H51 . 0.950 no
C6 . N4 . 1.349(8) yes
C6 . H61 . 0.950 no
C7 . N5 . 1.345(8) yes
C7 . N6 . 1.346(8) yes
C7 . H71 . 0.950 no
C8 . C9 . 1.360(8) yes
C8 . N6 . 1.352(8) yes
C8 . H81 . 0.950 no
C9 . N5 . 1.354(8) yes
C9 . H91 . 0.950 no
C10 . N7 . 1.343(8) yes
C10 . N8 . 1.343(8) yes
C10 . H101 . 0.950 no
C11 . C12 . 1.356(8) yes
C11 . N8 . 1.351(8) yes
C11 . H111 . 0.950 no
C12 . N7 . 1.355(9) yes
C12 . H121 . 0.950 no
C13 . N9 . 1.344(8) yes
C13 . N10 . 1.344(8) yes
C13 . H131 . 0.950 no
C14 . C15 . 1.358(8) yes
C14 . N10 . 1.351(8) yes
C14 . H141 . 0.950 no
C15 . N9 . 1.349(8) yes
C15 . H151 . 0.950 no
C16 . N11 . 1.346(8) yes
C16 . N12 . 1.343(8) yes
C16 . H161 . 0.950 no
C17 . C18 . 1.356(8) yes
C17 . N12 . 1.356(8) yes
C17 . H171 . 0.950 no
C18 . N11 . 1.352(8) yes
C18 . H181 . 0.950 no
C19 . N13 . 1.341(8) yes
C19 . N14 . 1.345(8) yes
C19 . H191 . 0.950 no
C20 . C21 . 1.358(8) yes
C20 . N13 . 1.354(8) yes
C20 . H201 . 0.950 no
C21 . N14 . 1.350(8) yes
C21 . H211 . 0.950 no
C22 . N15 . 1.346(8) yes
C22 . N16 . 1.346(8) yes
C22 . H221 . 0.950 no
C23 . C24 . 1.357(8) yes
C23 . N15 . 1.351(8) yes
C23 . H231 . 0.950 no
C24 . N16 . 1.354(8) yes
C24 . H241 . 0.950 no
C101 . N17 . 1.500(9) yes
C101 . H1011 . 0.960 no
C101 . H1012 . 0.960 no
C101 . H1013 . 0.960 no
C102 . N17 . 1.471(9) yes
C102 . H1021 . 0.960 no
C102 . H1022 . 0.960 no
C102 . H1023 . 0.960 no
C103 . N17 . 1.460(9) yes
C103 . O2 . 1.158(9) yes
C103 . H1031 . 0.980 no
C104 . N18 . 1.458(9) yes
C104 . O1 . 1.160(9) yes
C104 . H1041 . 0.980 no
C201 . N18 . 1.497(9) yes
C201 . H2011 . 0.960 no
C201 . H2012 . 0.960 no
C201 . H2013 . 0.960 no
C202 . N18 . 1.468(9) yes
C202 . H2021 . 0.960 no
C202 . H2022 . 0.960 no
C202 . H2023 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Zn1 . N3 . 112.9(19) yes
N1 . Zn1 . N5 . 111.8(15) yes
N3 . Zn1 . N5 . 114.6(14) yes
N1 . Zn1 . N7 . 110.1(7) yes
N3 . Zn1 . N7 . 101.0(17) yes
N5 . Zn1 . N7 . 105.7(17) yes
N8 4_565 Zn2 . N6 2_576 119.7(14) yes
N8 4_565 Zn2 . N4 . 113.1(17) yes
N6 2_576 Zn2 . N4 . 115.3(16) yes
N8 4_565 Zn2 . N9 . 100.5(20) yes
N6 2_576 Zn2 . N9 . 106.7(17) yes
N4 . Zn2 . N9 . 97.2(15) yes
N13 2_676 Zn3 . N11 1_556 109.9(13) yes
N13 2_676 Zn3 . N15 4_575 98.5(18) yes
N11 1_556 Zn3 . N15 4_575 114.9(20) yes
N13 2_676 Zn3 . N10 . 115.5(12) yes
N11 1_556 Zn3 . N10 . 108(2) yes
N15 4_575 Zn3 . N10 . 110.4(14) yes
N2 . Zn4 . N12 . 107.0(13) yes
N2 . Zn4 . N14 . 123(2) yes
N12 . Zn4 . N14 . 100.6(16) yes
N2 . Zn4 . N16 . 103.7(16) yes
N12 . Zn4 . N16 . 107.1(11) yes
N14 . Zn4 . N16 . 114.3(19) yes
N1 . C1 . N2 . 112.8(6) yes
N1 . C1 . H11 . 122.8 no
N2 . C1 . H11 . 124.4 no
C3 . C2 . N1 . 109.2(6) yes
C3 . C2 . H21 . 124.6 no
N1 . C2 . H21 . 126.1 no
C2 . C3 . N2 . 109.0(6) yes
C2 . C3 . H31 . 126.3 no
N2 . C3 . H31 . 124.7 no
N3 . C4 . N4 . 112.8(6) yes
N3 . C4 . H41 . 120.6 no
N4 . C4 . H41 . 126.5 no
C6 . C5 . N3 . 109.0(6) yes
C6 . C5 . H51 . 122.5 no
N3 . C5 . H51 . 128.5 no
C5 . C6 . N4 . 109.0(6) yes
C5 . C6 . H61 . 128.4 no
N4 . C6 . H61 . 122.5 no
N5 . C7 . N6 . 112.9(6) yes
N5 . C7 . H71 . 123.5 no
N6 . C7 . H71 . 123.5 no
C9 . C8 . N6 . 109.1(6) yes
C9 . C8 . H81 . 125.4 no
N6 . C8 . H81 . 125.4 no
C8 . C9 . N5 . 109.0(6) yes
C8 . C9 . H91 . 125.5 no
N5 . C9 . H91 . 125.4 no
N7 . C10 . N8 . 113.0(7) yes
N7 . C10 . H101 . 122.0 no
N8 . C10 . H101 . 125.0 no
C12 . C11 . N8 . 108.9(7) yes
C12 . C11 . H111 . 127.0 no
N8 . C11 . H111 . 124.0 no
C11 . C12 . N7 . 109.2(6) yes
C11 . C12 . H121 . 123.9 no
N7 . C12 . H121 . 126.9 no
N9 . C13 . N10 . 112.9(6) yes
N9 . C13 . H131 . 124.1 no
N10 . C13 . H131 . 123.0 no
C15 . C14 . N10 . 109.1(6) yes
C15 . C14 . H141 . 124.9 no
N10 . C14 . H141 . 125.9 no
C14 . C15 . N9 . 109.0(6) yes
C14 . C15 . H151 . 126.0 no
N9 . C15 . H151 . 125.0 no
N11 . C16 . N12 . 112.7(6) yes
N11 . C16 . H161 . 122.5 no
N12 . C16 . H161 . 124.9 no
C18 . C17 . N12 . 109.0(6) yes
C18 . C17 . H171 . 126.7 no
N12 . C17 . H171 . 124.3 no
C17 . C18 . N11 . 109.0(6) yes
C17 . C18 . H181 . 124.3 no
N11 . C18 . H181 . 126.7 no
N13 . C19 . N14 . 113.3(6) yes
N13 . C19 . H191 . 125.5 no
N14 . C19 . H191 . 121.2 no
C21 . C20 . N13 . 109.3(6) yes
C21 . C20 . H201 . 127.5 no
N13 . C20 . H201 . 123.2 no
C20 . C21 . N14 . 109.0(6) yes
C20 . C21 . H211 . 123.4 no
N14 . C21 . H211 . 127.7 no
N15 . C22 . N16 . 112.7(6) yes
N15 . C22 . H221 . 122.9 no
N16 . C22 . H221 . 124.4 no
C24 . C23 . N15 . 109.1(6) yes
C24 . C23 . H231 . 124.7 no
N15 . C23 . H231 . 126.2 no
C23 . C24 . N16 . 109.0(6) yes
C23 . C24 . H241 . 126.2 no
N16 . C24 . H241 . 124.7 no
N17 . C101 . H1011 . 108.0 no
N17 . C101 . H1012 . 103.8 no
H1011 . C101 . H1012 . 109.5 no
N17 . C101 . H1013 . 116.3 no
H1011 . C101 . H1013 . 109.5 no
H1012 . C101 . H1013 . 109.5 no
N17 . C102 . H1021 . 111.7 no
N17 . C102 . H1022 . 104.7 no
H1021 . C102 . H1022 . 109.5 no
N17 . C102 . H1023 . 111.8 no
H1021 . C102 . H1023 . 109.5 no
H1022 . C102 . H1023 . 109.5 no
N17 . C103 . O2 . 118.1(9) yes
N17 . C103 . H1031 . 110.9 no
O2 . C103 . H1031 . 123.8 no
N18 . C104 . O1 . 114(6) yes
N18 . C104 . H1041 . 116.8 no
O1 . C104 . H1041 . 127.5 no
N18 . C201 . H2011 . 112.4 no
N18 . C201 . H2012 . 104.8 no
H2011 . C201 . H2012 . 109.5 no
N18 . C201 . H2013 . 111.1 no
H2011 . C201 . H2013 . 109.5 no
H2012 . C201 . H2013 . 109.5 no
N18 . C202 . H2021 . 108.0 no
N18 . C202 . H2022 . 115.5 no
H2021 . C202 . H2022 . 109.5 no
N18 . C202 . H2023 . 104.8 no
H2021 . C202 . H2023 . 109.5 no
H2022 . C202 . H2023 . 109.5 no
C2 . N1 . C1 . 104.4(6) yes
C2 . N1 . Zn1 . 142(2) yes
C1 . N1 . Zn1 . 112(2) yes
C3 . N2 . C1 . 104.6(6) yes
C3 . N2 . Zn4 . 133(2) yes
C1 . N2 . Zn4 . 118(2) yes
C5 . N3 . C4 . 104.5(6) yes
C5 . N3 . Zn1 . 127(3) yes
C4 . N3 . Zn1 . 127(3) yes
C6 . N4 . C4 . 104.7(6) yes
C6 . N4 . Zn2 . 125(3) yes
C4 . N4 . Zn2 . 125(3) yes
C9 . N5 . C7 . 104.5(6) yes
C9 . N5 . Zn1 . 130(3) yes
C7 . N5 . Zn1 . 126(3) yes
C8 . N6 . C7 . 104.5(6) yes
C8 . N6 . Zn2 2_576 138(3) yes
C7 . N6 . Zn2 2_576 117(3) yes
C12 . N7 . C10 . 104.3(6) yes
C12 . N7 . Zn1 . 137(4) yes
C10 . N7 . Zn1 . 119(4) yes
C11 . N8 . C10 . 104.6(8) yes
C11 . N8 . Zn2 4_564 130(4) yes
C10 . N8 . Zn2 4_564 124(4) yes
C15 . N9 . C13 . 104.6(6) yes
C15 . N9 . Zn2 . 128(3) yes
C13 . N9 . Zn2 . 128(3) yes
C14 . N10 . C13 . 104.4(6) yes
C14 . N10 . Zn3 . 139(3) yes
C13 . N10 . Zn3 . 117(3) yes
C18 . N11 . C16 . 104.7(6) yes
C18 . N11 . Zn3 1_554 134(3) yes
C16 . N11 . Zn3 1_554 121(3) yes
C17 . N12 . C16 . 104.6(6) yes
C17 . N12 . Zn4 . 117(3) yes
C16 . N12 . Zn4 . 137(3) yes
C20 . N13 . C19 . 104.1(6) yes
C20 . N13 . Zn3 2_676 127(4) yes
C19 . N13 . Zn3 2_676 129(4) yes
C21 . N14 . C19 . 104.4(6) yes
C21 . N14 . Zn4 . 133(4) yes
C19 . N14 . Zn4 . 121(4) yes
C23 . N15 . C22 . 104.6(6) yes
C23 . N15 . Zn3 4_574 134(4) yes
C22 . N15 . Zn3 4_574 121(4) yes
C24 . N16 . C22 . 104.5(6) yes
C24 . N16 . Zn4 . 127(3) yes
C22 . N16 . Zn4 . 128(3) yes
C101 . N17 . C102 . 124.1(9) yes
C101 . N17 . C103 . 109.9(9) yes
C102 . N17 . C103 . 122.0(9) yes
C201 . N18 . C202 . 123.5(9) yes
C201 . N18 . C104 . 110.2(9) yes
C202 . N18 . C104 . 122.0(9) yes
# Attachment '- phaseI_13.cif'
data_phaseI_13
_database_code_depnum_ccdc_archive 'CCDC 828173'
#TrackingRef '- phaseI_13.cif'
_audit_creation_date 11-03-18
_audit_creation_method CRYSTALS_ver_14.06
_oxford_structure_analysis_title 'tst9008 in Pbca'
_chemical_name_systematic ?
_chemical_name_common ZIF-4
_chemical_formula_moiety 'C12 H12 N8 Zn2, C3 H7 N O'
# Given Formula = C10 H10 N5 O10 Zn0.50
# Dc = 1.23 Fooo = 1920.00 Mu = 6.53 M = 392.91
# Found Formula = C15 H19 N9 O1 Zn2
# Dc = 1.47 FOOO = 1920.00 Mu = 22.78 M = 472.14
_chemical_formula_sum 'C15 H19 N9 O1 Zn2'
_chemical_compound_source ?
_chemical_melting_point ?
_exptl_crystal_description block
_exptl_crystal_colour colourless
_diffrn_ambient_temperature 293
_diffrn_ambient_pressure 130
_publ_section_exptl_refinement
;
022_ALERT_3_A Ratio Unique / Expected Reflections too Low .... 0.65
026_ALERT_3_A Ratio Observed / Unique Reflections too Low .... 13 Perc.
027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 17.55 Deg.
029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.89
023_ALERT_3_B Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.40 Deg.
341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 25
911_ALERT_3_B Missing # FCF Refl Between THmin & STh/L= 0.559 882
088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.16
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 8
913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5
860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 240
950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 2
952_ALERT_1_C Reported and Calculated Lmax Values Differ by .. 2
234_ALERT_4_C Large Hirshfeld Difference Zn1 -- N2 .. 0.17 Ang.
234_ALERT_4_C Large Hirshfeld Difference Zn1 -- N8 .. 0.15 Ang.
All of the above are caused by shading from the pressure cell. 1,2 and 1,3
restraints were applied to all non-hydrogen distamces.
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5
241_ALERT_2_C Check High Ueq as Compared to Neighbors for C8
242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3
244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of N9
All of the above are caused by DMF solvent. This molecule was restrained to
low temperature values, while thermal similarity restraints were applied
to all non-hydrigen atoms.
380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C15
This is correct.
731_ALERT_1_B Bond Calc 1.47(4), Rep 1.469(9) ...... 4.44 su-Ra
N9 -C13 1.555 1.555
731_ALERT_1_B Bond Calc 1.49(5), Rep 1.495(9) ...... 5.56 su-Ra
N9 -C14 1.555 1.555
731_ALERT_1_B Bond Calc 1.46(5), Rep 1.457(9) ...... 5.56 su-Ra
N9 -C15 1.555 1.555
731_ALERT_1_B Bond Calc 1.16(5), Rep 1.155(9) ...... 5.56 su-Ra
C13 -O1 1.555 1.555
731_ALERT_1_C Bond Calc 1.307(17), Rep 1.308(8) ...... 2.13 su-Ra
N1 -C1 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.321(9) ...... 2.22 su-Ra
N1 -C3 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.315(8) ...... 2.50 su-Ra
N2 -C1 1.555 1.555
731_ALERT_1_C Bond Calc 1.316(18), Rep 1.316(8) ...... 2.25 su-Ra
N2 -C2 1.555 1.555
731_ALERT_1_C Bond Calc 1.308(18), Rep 1.308(8) ...... 2.25 su-Ra
N3 -C4 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(3), Rep 1.318(9) ...... 3.33 su-Ra
N3 -C6 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.317(8) ...... 2.50 su-Ra
N4 -C4 1.555 1.555
731_ALERT_1_C Bond Calc 1.31(2), Rep 1.309(8) ...... 2.50 su-Ra
N4 -C5 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.315(8) ...... 2.50 su-Ra
N5 -C7 1.555 1.555
731_ALERT_1_C Bond Calc 1.31(2), Rep 1.312(8) ...... 2.50 su-Ra
N5 -C9 1.555 1.555
731_ALERT_1_C Bond Calc 1.31(2), Rep 1.310(8) ...... 2.50 su-Ra
N6 -C7 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.318(8) ...... 2.50 su-Ra
N6 -C8 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.316(9) ...... 2.22 su-Ra
N7 -C10 1.555 1.555
731_ALERT_1_C Bond Calc 1.31(2), Rep 1.311(9) ...... 2.22 su-Ra
N7 -C11 1.555 1.555
731_ALERT_1_C Bond Calc 1.31(2), Rep 1.315(8) ...... 2.50 su-Ra
N8 -C10 1.555 1.555
731_ALERT_1_C Bond Calc 1.32(2), Rep 1.317(9) ...... 2.22 su-Ra
N8 -C12 1.555 1.555
731_ALERT_1_C Bond Calc 1.35(2), Rep 1.353(9) ...... 2.22 su-Ra
C2 -C3 1.555 1.555
731_ALERT_1_C Bond Calc 1.35(2), Rep 1.352(9) ...... 2.22 su-Ra
C5 -C6 1.555 1.555
731_ALERT_1_C Bond Calc 1.35(3), Rep 1.348(9) ...... 3.33 su-Ra
C8 -C9 1.555 1.555
731_ALERT_1_C Bond Calc 1.35(3), Rep 1.349(9) ...... 3.33 su-Ra
C11 -C12 1.555 1.555
732_ALERT_1_C Angle Calc 104.7(13), Rep 104.6(6) ...... 2.17 su-Ra
C1 -N1 -C3 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 103.0(13), Rep 103.1(6) ...... 2.17 su-Ra
C4 -N4 -C5 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 103.1(15), Rep 103.2(6) ...... 2.50 su-Ra
C7 -N5 -C9 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 103.5(14), Rep 103.5(6) ...... 2.33 su-Ra
C7 -N6 -C8 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 104.2(14), Rep 104.2(6) ...... 2.33 su-Ra
C10 -N7 -C11 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 103.7(14), Rep 103.6(6) ...... 2.33 su-Ra
C10 -N8 -C12 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 113.7(13), Rep 113.7(6) ...... 2.17 su-Ra
N2 -C1 -N1 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 108.9(15), Rep 108.9(6) ...... 2.50 su-Ra
N2 -C2 -C3 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 115.0(15), Rep 114.9(6) ...... 2.50 su-Ra
N4 -C4 -N3 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 109.9(18), Rep 109.8(6) ...... 3.00 su-Ra
N4 -C5 -C6 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 108.5(15), Rep 108.4(6) ...... 2.50 su-Ra
C5 -C6 -N3 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 115.0(13), Rep 114.9(6) ...... 2.17 su-Ra
N5 -C7 -N6 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 108.6(16), Rep 108.7(6) ...... 2.67 su-Ra
N6 -C8 -C9 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 109.6(15), Rep 109.6(6) ...... 2.50 su-Ra
C8 -C9 -N5 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 114.1(14), Rep 114.0(6) ...... 2.33 su-Ra
N7 -C10 -N8 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 108.7(14), Rep 108.8(6) ...... 2.33 su-Ra
N7 -C11 -C12 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 109.2(14), Rep 109.3(6) ...... 2.33 su-Ra
C11 -C12 -N8 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 111(3), Rep 110.2(9) ...... 3.33 su-Ra
C13 -N9 -C14 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 125(3), Rep 124.8(9) ...... 3.33 su-Ra
C13 -N9 -C15 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 123(3), Rep 122.9(9) ...... 3.33 su-Ra
C14 -N9 -C15 1.555 1.555 1.555
732_ALERT_1_C Angle Calc 118(3), Rep 117.8(9) ...... 3.33 su-Ra
N9 -C13 -O1 1.555 1.555 1.555
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 is badly in error.
199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
This is correct.
760_ALERT_1_G CIF Contains no Torsion Angles ................. ?
No action taken.
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found ?
A shelx weighting scheme was not used.
;
_publ_section_exptl_prep
# Brief details or a reference. Include solvent if known
;
?
;
#end of refcif
_cell_length_a 15.3486(14)
_cell_length_b 15.1069(17)
_cell_length_c 18.3430(19)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4253.2(8)
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_H-M 'P b c a'
_symmetry_int_tables_number 61
# 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 .
_symmetry_space_group_name_Hall '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 8
_chemical_formula_weight 472.14
_cell_measurement_reflns_used 2065
_cell_measurement_theta_min 3
_cell_measurement_theta_max 23
_cell_measurement_temperature 293
_exptl_crystal_size_min 0.140
_exptl_crystal_size_mid 0.170
_exptl_crystal_size_max 0.220
_exptl_crystal_density_diffrn 1.475
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1920
_exptl_absorpt_coefficient_mu 2.278
# Sheldrick geometric approximatio 0.68 0.73
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min 0.58
_exptl_absorpt_correction_T_max 0.73
_diffrn_measurement_device_type 'Bruker SMART'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed X-ray tube'
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'SMART (Siemens, 1993)'
_computing_cell_refinement 'SAINT (Siemens ,1995)'
_computing_data_reduction 'SAINT (Siemens ,1995)'
_computing_structure_solution 'USER DEFINED 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_reflns_number 11913
_reflns_number_total 2025
_diffrn_reflns_av_R_equivalents 0.000
# Number of reflections without Friedels Law is 2428
# Number of reflections with Friedels Law is 2025
# Theoretical number of reflections is about 3109
_diffrn_reflns_theta_min 2.916
_diffrn_reflns_theta_max 23.400
_diffrn_measured_fraction_theta_max 0.651
_diffrn_reflns_theta_full 17.550
_diffrn_measured_fraction_theta_full 0.887
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 17
_reflns_limit_h_min 0
_reflns_limit_h_max 15
_reflns_limit_k_min 0
_reflns_limit_k_max 14
_reflns_limit_l_min 0
_reflns_limit_l_max 17
_oxford_diffrn_Wilson_B_factor 5.06
_oxford_diffrn_Wilson_scale 423.22
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.89
_refine_diff_density_max 0.90
# 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>-10.0\s(I)
_refine_ls_number_reflns 1990
_refine_ls_number_restraints 240
_refine_ls_number_parameters 244
_oxford_refine_ls_R_factor_ref 0.1810
_refine_ls_wR_factor_ref 0.2249
_refine_ls_goodness_of_fit_ref 0.8034
_refine_ls_shift/su_max 0.0001219
# The values computed from all data
_oxford_reflns_number_all 1990
_refine_ls_R_factor_all 0.1810
_refine_ls_wR_factor_all 0.2249
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 262
_refine_ls_R_factor_gt 0.0559
_refine_ls_wR_factor_gt 0.0946
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.34 0.979 -0.133
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
User-defined structure solution reference
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Prince, E.
Mathematical Techniques in Crystallography
and Materials Science
Springer-Verlag, New York, 1982.
Siemens Industrial Automation, Inc (1993).
SMART: Area-Detector Software Package; Madison, WI.
Siemens Industrial Automation, Inc (1995).
SAINT: Area-Detector Integration Software.; Madison, WI.
Siemens Industrial Automation, Inc (1996).
SADABS: Area-Detector Absorption Correction;: Madison, WI.
Watkin D.J. (1994).
Acta Cryst, A50, 411-437.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atomsattached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Zn1 Zn 0.20565(15) 0.13848(17) 0.40844(13) 0.0737 1.0000 Uani . . . . . . .
Zn2 Zn 0.51268(15) 0.33706(17) 0.31330(13) 0.0732 1.0000 Uani . . . . . . .
N1 N 0.4461(8) 0.2344(10) 0.3538(8) 0.0765 1.0000 Uani D U . . . . .
N2 N 0.3306(6) 0.1608(9) 0.3901(9) 0.0756 1.0000 Uani D U . . . . .
N3 N 0.1058(8) 0.1310(11) 0.6165(6) 0.0758 1.0000 Uani D U . . . . .
N4 N 0.1790(10) 0.1225(13) 0.5127(6) 0.0886 1.0000 Uani D U . . . . .
N5 N 0.0759(9) -0.0669(10) 0.3053(8) 0.0781 1.0000 Uani D U . . . . .
N6 N 0.1630(10) 0.0369(10) 0.3492(7) 0.0741 1.0000 Uani D U . . . . .
N7 N 0.0644(11) 0.3127(10) 0.2824(7) 0.0852 1.0000 Uani D U . . . . .
N8 N 0.1395(10) 0.2406(9) 0.3660(7) 0.0737 1.0000 Uani D U . . . . .
C1 C 0.3614(8) 0.2341(10) 0.3611(10) 0.0742 1.0000 Uani D U . . . . .
C2 C 0.4004(9) 0.1135(10) 0.4048(12) 0.0958 1.0000 Uani D U . . . . .
C3 C 0.4718(7) 0.1586(12) 0.3826(12) 0.0909 1.0000 Uani D U . . . . .
C4 C 0.1096(10) 0.1520(13) 0.5474(7) 0.0797 1.0000 Uani D U . . . . .
C5 C 0.2223(12) 0.0812(18) 0.5639(9) 0.1219 1.0000 Uani D U . . . . .
C6 C 0.1790(13) 0.0874(18) 0.6278(7) 0.1147 1.0000 Uani D U . . . . .
C7 C 0.0966(11) -0.0157(12) 0.3606(7) 0.0785 1.0000 Uani D U . . . . .
C8 C 0.1898(12) 0.0146(14) 0.2834(9) 0.1051 1.0000 Uani D U . . . . .
C9 C 0.1353(13) -0.0473(14) 0.2564(8) 0.0997 1.0000 Uani D U . . . . .
C10 C 0.1033(13) 0.2385(10) 0.3011(8) 0.0870 1.0000 Uani D U . . . . .
C11 C 0.0791(16) 0.3661(9) 0.3374(10) 0.1060 1.0000 Uani D U . . . . .
C12 C 0.1217(15) 0.3208(11) 0.3899(8) 0.1001 1.0000 Uani D U . . . . .
N9 N 0.8223(18) 0.1775(18) 0.3981(16) 0.2111 1.0000 Uani D U . . . . .
C13 C 0.7287(19) 0.162(3) 0.3868(17) 0.2335 1.0000 Uani D U . . . . .
C14 C 0.867(3) 0.192(3) 0.327(2) 0.3382 1.0000 Uani D U . . . . .
C15 C 0.869(2) 0.157(4) 0.465(2) 0.3635 1.0000 Uani D U . . . . .
O1 O 0.6902(16) 0.128(2) 0.4332(17) 0.2638 1.0000 Uani D U . . . . .
H11 H 0.3261 0.2811 0.3469 0.0888 1.0000 Uiso R . . . . . .
H21 H 0.4007 0.0582 0.4271 0.1151 1.0000 Uiso R . . . . . .
H31 H 0.5291 0.1394 0.3866 0.1092 1.0000 Uiso R . . . . . .
H41 H 0.0668 0.1855 0.5244 0.0956 1.0000 Uiso R . . . . . .
H51 H 0.2752 0.0523 0.5573 0.1461 1.0000 Uiso R . . . . . .
H61 H 0.1973 0.0643 0.6723 0.1374 1.0000 Uiso R . . . . . .
H71 H 0.0662 -0.0168 0.4045 0.0943 1.0000 Uiso R . . . . . .
H81 H 0.2384 0.0376 0.2598 0.1261 1.0000 Uiso R . . . . . .
H91 H 0.1391 -0.0719 0.2100 0.1197 1.0000 Uiso R . . . . . .
H101 H 0.1054 0.1890 0.2710 0.1045 1.0000 Uiso R . . . . . .
H111 H 0.0633 0.4254 0.3396 0.1272 1.0000 Uiso R . . . . . .
H121 H 0.1358 0.3428 0.4358 0.1203 1.0000 Uiso R . . . . . .
H131 H 0.7013 0.1794 0.3439 0.2806 1.0000 Uiso R . . . . . .
H141 H 0.9279 0.2014 0.3344 0.4067 1.0000 Uiso R . . . . . .
H142 H 0.8420 0.2424 0.3028 0.4067 1.0000 Uiso R . . . . . .
H143 H 0.8589 0.1404 0.2963 0.4067 1.0000 Uiso R . . . . . .
H151 H 0.9296 0.1728 0.4590 0.4368 1.0000 Uiso R . . . . . .
H152 H 0.8450 0.1903 0.5047 0.4368 1.0000 Uiso R . . . . . .
H153 H 0.8648 0.0950 0.4751 0.4368 1.0000 Uiso R . . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0627(18) 0.0884(19) 0.0701(17) 0.0032(13) 0.0024(11) -0.0043(13)
Zn2 0.0603(17) 0.092(2) 0.0676(16) -0.0014(13) 0.0049(12) 0.0012(12)
N1 0.043(7) 0.099(12) 0.087(11) 0.003(8) 0.020(8) -0.004(6)
N2 0.031(7) 0.071(11) 0.124(12) -0.008(9) 0.001(8) -0.003(5)
N3 0.055(9) 0.107(13) 0.065(8) 0.005(8) -0.007(6) 0.015(8)
N4 0.071(12) 0.136(15) 0.059(8) 0.019(9) -0.004(6) 0.022(9)
N5 0.080(11) 0.081(12) 0.073(10) 0.001(8) 0.016(7) -0.016(7)
N6 0.067(11) 0.100(13) 0.055(8) 0.006(7) 0.001(7) -0.015(7)
N7 0.095(13) 0.084(12) 0.077(10) 0.015(7) -0.027(8) -0.009(8)
N8 0.072(11) 0.078(10) 0.070(9) 0.005(7) -0.007(7) 0.014(8)
C1 0.039(7) 0.092(12) 0.091(13) 0.008(10) 0.002(9) 0.000(7)
C2 0.041(10) 0.101(12) 0.146(16) 0.028(12) 0.031(11) 0.018(7)
C3 0.036(7) 0.104(14) 0.132(16) 0.008(12) 0.022(11) 0.009(7)
C4 0.068(12) 0.109(16) 0.063(9) 0.001(10) -0.015(7) 0.020(9)
C5 0.097(15) 0.20(2) 0.072(11) 0.041(14) 0.014(9) 0.074(13)
C6 0.090(15) 0.19(2) 0.063(9) 0.027(13) 0.003(9) 0.068(13)
C7 0.065(13) 0.100(15) 0.071(10) -0.008(9) 0.023(8) -0.010(8)
C8 0.117(16) 0.115(17) 0.083(12) -0.012(10) 0.046(10) -0.048(11)
C9 0.108(16) 0.111(17) 0.081(11) -0.024(10) 0.039(10) -0.030(10)
C10 0.096(15) 0.096(12) 0.069(11) -0.012(9) -0.011(10) 0.023(11)
C11 0.127(17) 0.075(11) 0.116(15) -0.005(8) -0.057(13) 0.019(12)
C12 0.129(17) 0.074(12) 0.098(12) -0.011(9) -0.055(12) 0.010(11)
N9 0.27(3) 0.18(2) 0.19(3) 0.00(2) 0.02(2) 0.08(3)
C13 0.26(3) 0.20(3) 0.24(3) 0.02(3) 0.03(3) 0.09(3)
C14 0.41(5) 0.30(5) 0.30(4) 0.08(5) 0.13(4) -0.05(5)
C15 0.44(5) 0.38(6) 0.27(4) -0.03(5) -0.11(4) 0.09(5)
O1 0.27(3) 0.28(4) 0.24(3) 0.01(3) 0.08(2) 0.10(3)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.036855(14)
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
Zn1 . N2 . 1.976(10) yes
Zn1 . N4 . 1.971(11) yes
Zn1 . N6 . 1.991(11) yes
Zn1 . N8 . 2.004(11) yes
Zn2 . N5 3_555 1.994(11) yes
Zn2 . N3 4_556 1.984(11) yes
Zn2 . N7 8_555 1.961(11) yes
Zn2 . N1 . 2.000(11) yes
N1 . C1 . 1.308(8) yes
N1 . C3 . 1.321(9) yes
N2 . C1 . 1.315(8) yes
N2 . C2 . 1.316(8) yes
N3 . C4 . 1.308(8) yes
N3 . C6 . 1.318(9) yes
N4 . C4 . 1.317(8) yes
N4 . C5 . 1.309(8) yes
N5 . C7 . 1.315(8) yes
N5 . C9 . 1.312(8) yes
N6 . C7 . 1.310(8) yes
N6 . C8 . 1.318(8) yes
N7 . C10 . 1.316(9) yes
N7 . C11 . 1.311(9) yes
N8 . C10 . 1.315(8) yes
N8 . C12 . 1.317(9) yes
C1 . H11 . 0.930 no
C2 . C3 . 1.353(9) yes
C2 . H21 . 0.930 no
C3 . H31 . 0.930 no
C4 . H41 . 0.930 no
C5 . C6 . 1.352(9) yes
C5 . H51 . 0.930 no
C6 . H61 . 0.930 no
C7 . H71 . 0.930 no
C8 . C9 . 1.348(9) yes
C8 . H81 . 0.930 no
C9 . H91 . 0.930 no
C10 . H101 . 0.930 no
C11 . C12 . 1.349(9) yes
C11 . H111 . 0.930 no
C12 . H121 . 0.930 no
N9 . C13 . 1.469(9) yes
N9 . C14 . 1.495(9) yes
N9 . C15 . 1.457(9) yes
C13 . O1 . 1.155(9) yes
C13 . H131 . 0.930 no
C14 . H141 . 0.960 no
C14 . H142 . 0.960 no
C14 . H143 . 0.960 no
C15 . H151 . 0.960 no
C15 . H152 . 0.960 no
C15 . H153 . 0.960 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Zn1 . N4 . 112.8(7) yes
N2 . Zn1 . N6 . 111.0(6) yes
N4 . Zn1 . N6 . 111.5(7) yes
N2 . Zn1 . N8 . 107.1(6) yes
N4 . Zn1 . N8 . 111.5(6) yes
N6 . Zn1 . N8 . 102.4(6) yes
N5 3_555 Zn2 . N3 4_556 111.2(7) yes
N5 3_555 Zn2 . N7 8_555 110.3(6) yes
N3 4_556 Zn2 . N7 8_555 109.6(7) yes
N5 3_555 Zn2 . N1 . 104.1(6) yes
N3 4_556 Zn2 . N1 . 108.4(6) yes
N7 8_555 Zn2 . N1 . 113.2(7) yes
Zn2 . N1 . C1 . 123.3(10) yes
Zn2 . N1 . C3 . 131.9(10) yes
C1 . N1 . C3 . 104.6(6) yes
Zn1 . N2 . C1 . 124.1(9) yes
Zn1 . N2 . C2 . 131.5(9) yes
C1 . N2 . C2 . 104.3(6) yes
Zn2 4_456 N3 . C4 . 127.0(9) yes
Zn2 4_456 N3 . C6 . 129.2(9) yes
C4 . N3 . C6 . 103.7(6) yes
Zn1 . N4 . C4 . 126.5(9) yes
Zn1 . N4 . C5 . 130.4(9) yes
C4 . N4 . C5 . 103.1(6) yes
Zn2 3_545 N5 . C7 . 122.3(9) yes
Zn2 3_545 N5 . C9 . 133.5(10) yes
C7 . N5 . C9 . 103.2(6) yes
Zn1 . N6 . C7 . 129.5(10) yes
Zn1 . N6 . C8 . 126.5(9) yes
C7 . N6 . C8 . 103.5(6) yes
Zn2 8_455 N7 . C10 . 125.2(10) yes
Zn2 8_455 N7 . C11 . 130.0(10) yes
C10 . N7 . C11 . 104.2(6) yes
Zn1 . N8 . C10 . 123.2(9) yes
Zn1 . N8 . C12 . 133.2(10) yes
C10 . N8 . C12 . 103.6(6) yes
N2 . C1 . N1 . 113.7(6) yes
N2 . C1 . H11 . 123.1 no
N1 . C1 . H11 . 123.2 no
N2 . C2 . C3 . 108.9(6) yes
N2 . C2 . H21 . 125.6 no
C3 . C2 . H21 . 125.5 no
C2 . C3 . N1 . 108.4(6) yes
C2 . C3 . H31 . 125.8 no
N1 . C3 . H31 . 125.8 no
N4 . C4 . N3 . 114.9(6) yes
N4 . C4 . H41 . 122.5 no
N3 . C4 . H41 . 122.6 no
N4 . C5 . C6 . 109.8(6) yes
N4 . C5 . H51 . 125.1 no
C6 . C5 . H51 . 125.1 no
C5 . C6 . N3 . 108.4(6) yes
C5 . C6 . H61 . 125.8 no
N3 . C6 . H61 . 125.7 no
N5 . C7 . N6 . 114.9(6) yes
N5 . C7 . H71 . 122.5 no
N6 . C7 . H71 . 122.7 no
N6 . C8 . C9 . 108.7(6) yes
N6 . C8 . H81 . 125.5 no
C9 . C8 . H81 . 125.7 no
C8 . C9 . N5 . 109.6(6) yes
C8 . C9 . H91 . 125.1 no
N5 . C9 . H91 . 125.3 no
N7 . C10 . N8 . 114.0(6) yes
N7 . C10 . H101 . 123.0 no
N8 . C10 . H101 . 122.9 no
N7 . C11 . C12 . 108.8(6) yes
N7 . C11 . H111 . 125.6 no
C12 . C11 . H111 . 125.7 no
C11 . C12 . N8 . 109.3(6) yes
C11 . C12 . H121 . 125.3 no
N8 . C12 . H121 . 125.4 no
C13 . N9 . C14 . 110.2(9) yes
C13 . N9 . C15 . 124.8(9) yes
C14 . N9 . C15 . 122.9(9) yes
N9 . C13 . O1 . 117.8(9) yes
N9 . C13 . H131 . 121.2 no
O1 . C13 . H131 . 121.0 no
N9 . C14 . H141 . 109.6 no
N9 . C14 . H142 . 109.3 no
H141 . C14 . H142 . 109.5 no
N9 . C14 . H143 . 109.5 no
H141 . C14 . H143 . 109.5 no
H142 . C14 . H143 . 109.5 no
N9 . C15 . H151 . 109.3 no
N9 . C15 . H152 . 109.7 no
H151 . C15 . H152 . 109.5 no
N9 . C15 . H153 . 109.4 no
H151 . C15 . H153 . 109.5 no
H152 . C15 . H153 . 109.5 no