# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_z
_database_code_depnum_ccdc_archive 'CCDC 1538298'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-05-04 downloaded from the CCDC.
;
_audit_creation_date 2017-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'Cd I4, 2(C8 H12 N)'
_chemical_formula_sum 'C16 H24 Cd I4 N2'
_chemical_formula_weight 864.37
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 11
_space_group_name_H-M_alt 'P 1 21/m 1'
_space_group_name_Hall '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
_cell_length_a 10.8728(17)
_cell_length_b 8.4539(11)
_cell_length_c 13.6191(18)
_cell_angle_alpha 90
_cell_angle_beta 98.521(4)
_cell_angle_gamma 90
_cell_volume 1238.0(3)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6518
_cell_measurement_temperature 320(2)
_cell_measurement_theta_max 27.45
_cell_measurement_theta_min 3.02
_shelx_estimated_absorpt_T_max 1.000
_shelx_estimated_absorpt_T_min 0.273
_exptl_absorpt_coefficient_mu 5.870
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ABSCOR
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.319
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 788
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max 1.000000
_exptl_transmission_factor_min 0.273454
_diffrn_reflns_av_R_equivalents 0.0563
_diffrn_reflns_av_unetI/netI 0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 6876
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.995
_diffrn_reflns_theta_min 3.025
_diffrn_ambient_temperature 320(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type 'multiwire proportional'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2101
_reflns_number_total 2538
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 1.145
_refine_diff_density_min -2.148
_refine_diff_density_rms 0.322
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.221
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 171
_refine_ls_number_reflns 2538
_refine_ls_number_restraints 118
_refine_ls_R_factor_all 0.0820
_refine_ls_R_factor_gt 0.0704
_refine_ls_restrained_S_all 1.202
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+8.8105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1979
_refine_ls_wR_factor_ref 0.2099
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
C9-C10 = C10-C11 = C1-C2 = C2-C3
1.5 with sigma of 0.02
N1-C1 = N2-C9
1.47 with sigma of 0.02
N1-C2 = C1-C3 = N2-C10 = C9-C11
2.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim N2 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15
\\sim C16: within 1.6A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
Fixed Sof: I3(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5) H1D(0.5)
H1E(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5)
C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) N2(0.5) H2C(0.5) H2D(0.5)
H2E(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5)
C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5)
C16(0.5) H16(0.5)
5.a Secondary CH2 refined with riding coordinates:
C1(H1D,H1E), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16)
5.c Fitted hexagon refined as free rotating group:
C3(C4,C5,C6,C7,C8), C11(C12,C13,C14,C15,C16)
5.d Idealised Me refined as rotating group:
N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.29090(14) 0.250000 0.66117(10) 0.0886(5) Uani 1 2 d S T P A .
I2 I 0.33193(10) -0.01356(10) 0.38163(7) 0.0770(4) Uani 1 1 d . . . . .
Cd1 Cd 0.22717(13) 0.250000 0.45768(10) 0.0619(4) Uani 1 2 d S T P . .
I3 I -0.02983(17) 0.2183(6) 0.40214(12) 0.0791(16) Uani 0.5 1 d . . . A -1
N1 N -0.044(2) 0.276(5) 0.6617(11) 0.077(10) Uani 0.5 1 d D U . B -1
H1A H 0.019702 0.310021 0.633660 0.093 Uiso 0.5 1 calc GR . . B -1
H1B H -0.112567 0.328919 0.636579 0.093 Uiso 0.5 1 calc GR . . B -1
H1C H -0.055862 0.173185 0.649500 0.093 Uiso 0.5 1 calc GR . . B -1
C1 C -0.019(2) 0.302(3) 0.7688(12) 0.072(7) Uani 0.5 1 d D U . B -1
H1D H -0.091410 0.350496 0.789556 0.086 Uiso 0.5 1 calc R . . B -1
H1E H 0.049031 0.377382 0.781949 0.086 Uiso 0.5 1 calc R . . B -1
C2 C 0.015(2) 0.160(3) 0.8323(13) 0.073(6) Uani 0.5 1 d D U . B -1
H2A H 0.071022 0.094293 0.801126 0.088 Uiso 0.5 1 calc R . . B -1
H2B H -0.060164 0.098766 0.835412 0.088 Uiso 0.5 1 calc R . . B -1
C3 C 0.0742(15) 0.197(2) 0.9358(8) 0.069(5) Uani 0.5 1 d D U . B -1
C4 C 0.1868(15) 0.277(3) 0.9575(12) 0.084(6) Uani 0.5 1 d G U . B -1
H4 H 0.232114 0.301905 0.906816 0.101 Uiso 0.5 1 calc R . . B -1
C5 C 0.2318(16) 0.318(3) 1.0549(14) 0.097(7) Uani 0.5 1 d G U . B -1
H5 H 0.307211 0.371567 1.069431 0.116 Uiso 0.5 1 calc R . . B -1
C6 C 0.164(2) 0.281(3) 1.1307(10) 0.097(8) Uani 0.5 1 d G U . B -1
H6 H 0.194268 0.308558 1.195847 0.116 Uiso 0.5 1 calc R . . B -1
C7 C 0.052(2) 0.201(2) 1.1090(10) 0.088(7) Uani 0.5 1 d G U . B -1
H7 H 0.006228 0.175885 1.159648 0.106 Uiso 0.5 1 calc R . . B -1
C8 C 0.0065(15) 0.159(2) 1.0115(12) 0.082(6) Uani 0.5 1 d G U . B -1
H8 H -0.068871 0.106221 0.997033 0.099 Uiso 0.5 1 calc R . . B -1
N2 N 0.607(2) 0.235(9) 0.3748(11) 0.085(9) Uani 0.5 1 d D U . C -1
H2C H 0.668589 0.165105 0.385420 0.102 Uiso 0.5 1 calc GR . . C -1
H2D H 0.537959 0.193083 0.391159 0.102 Uiso 0.5 1 calc GR . . C -1
H2E H 0.627410 0.320957 0.411723 0.102 Uiso 0.5 1 calc GR . . C -1
C9 C 0.586(3) 0.280(5) 0.2697(14) 0.104(9) Uani 0.5 1 d D U . C -1
H9A H 0.611414 0.389178 0.264571 0.124 Uiso 0.5 1 calc R . . C -1
H9B H 0.497598 0.274580 0.246420 0.124 Uiso 0.5 1 calc R . . C -1
C10 C 0.652(4) 0.183(4) 0.2005(15) 0.106(8) Uani 0.5 1 d D U . C -1
H10A H 0.617867 0.076578 0.195714 0.127 Uiso 0.5 1 calc R . . C -1
H10B H 0.739524 0.176382 0.226116 0.127 Uiso 0.5 1 calc R . . C -1
C11 C 0.634(2) 0.261(4) 0.0972(9) 0.100(6) Uani 0.5 1 d D U . C -1
C12 C 0.712(2) 0.159(3) 0.0557(15) 0.109(8) Uani 0.5 1 d G U . C -1
H12 H 0.774447 0.104685 0.096386 0.131 Uiso 0.5 1 calc R . . C -1
C13 C 0.699(2) 0.140(3) -0.0467(16) 0.106(8) Uani 0.5 1 d G U . C -1
H13 H 0.751271 0.071865 -0.074490 0.128 Uiso 0.5 1 calc R . . C -1
C14 C 0.606(2) 0.221(3) -0.1075(10) 0.085(7) Uani 0.5 1 d G U . C -1
H14 H 0.596493 0.208135 -0.176047 0.102 Uiso 0.5 1 calc R . . C -1
C15 C 0.527(2) 0.323(3) -0.0660(13) 0.089(7) Uani 0.5 1 d G U . C -1
H15 H 0.464890 0.377227 -0.106729 0.106 Uiso 0.5 1 calc R . . C -1
C16 C 0.541(2) 0.342(3) 0.0364(14) 0.093(7) Uani 0.5 1 d G U . C -1
H16 H 0.488063 0.410049 0.064147 0.112 Uiso 0.5 1 calc R . . C -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0635(9) 0.1449(14) 0.0550(7) 0.000 0.0007(6) 0.000
I2 0.0809(7) 0.0604(5) 0.0882(7) -0.0103(4) 0.0079(5) 0.0044(4)
Cd1 0.0591(8) 0.0667(8) 0.0591(7) 0.000 0.0061(5) 0.000
I3 0.0555(8) 0.119(5) 0.0602(8) -0.0144(12) 0.0013(6) 0.0062(11)
N1 0.070(12) 0.10(3) 0.055(9) 0.005(13) -0.003(8) 0.010(17)
C1 0.052(12) 0.105(18) 0.061(11) 0.005(10) 0.014(10) 0.008(10)
C2 0.046(11) 0.106(14) 0.072(11) 0.014(11) 0.021(10) 0.011(10)
C3 0.049(9) 0.094(13) 0.069(10) 0.006(9) 0.022(8) 0.006(8)
C4 0.062(11) 0.106(16) 0.084(11) -0.003(13) 0.012(9) 0.001(12)
C5 0.082(14) 0.104(16) 0.097(14) -0.011(13) -0.010(12) 0.004(12)
C6 0.111(15) 0.097(17) 0.078(12) -0.002(12) -0.006(12) 0.013(13)
C7 0.108(15) 0.092(16) 0.069(11) -0.001(10) 0.029(11) 0.013(11)
C8 0.079(13) 0.094(14) 0.078(12) 0.010(11) 0.025(10) 0.008(11)
N2 0.069(12) 0.12(3) 0.069(10) -0.01(2) 0.019(8) 0.02(3)
C9 0.100(16) 0.13(2) 0.081(13) -0.007(15) 0.004(12) 0.033(17)
C10 0.104(15) 0.129(18) 0.084(13) -0.002(13) 0.014(12) 0.042(14)
C11 0.094(13) 0.128(14) 0.078(10) 0.002(14) 0.010(9) 0.014(15)
C12 0.095(16) 0.124(16) 0.107(14) 0.015(15) 0.011(13) 0.001(14)
C13 0.110(16) 0.098(16) 0.113(15) 0.010(14) 0.022(14) 0.000(14)
C14 0.090(14) 0.077(17) 0.092(13) 0.007(12) 0.022(10) -0.008(12)
C15 0.092(15) 0.084(13) 0.092(13) 0.011(12) 0.019(12) -0.003(12)
C16 0.093(15) 0.101(14) 0.087(13) -0.001(13) 0.017(12) 0.012(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cd1 2.7553(19) . ?
I2 Cd1 2.7720(13) . ?
Cd1 I3 2.797(2) . ?
N1 C1 1.461(17) . ?
C1 C2 1.493(17) . ?
C2 C3 1.494(17) . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
N2 C9 1.465(19) . ?
C9 C10 1.503(18) . ?
C10 C11 1.538(18) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Cd1 I2 108.65(4) . . ?
I1 Cd1 I2 108.65(4) . 4_565 ?
I1 Cd1 I3 111.36(7) . . ?
I2 Cd1 I2 106.99(7) . 4_565 ?
I2 Cd1 I3 105.74(10) . . ?
I2 Cd1 I3 115.16(10) 4_565 . ?
N1 C1 C2 116.9(19) . . ?
C1 C2 C3 114.2(16) . . ?
C4 C3 C2 123.2(14) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 C2 116.6(15) . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C7 C8 C3 120.0 . . ?
N2 C9 C10 117(2) . . ?
C9 C10 C11 109.5(16) . . ?
C12 C11 C10 96.1(16) . . ?
C12 C11 C16 120.0 . . ?
C16 C11 C10 137.7(18) . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
_shelx_res_file
;
TITL z in P2(1)/m
z.res
created by SHELXL-2016/6 at 16:41:14 on 05-Mar-2017
CELL 0.71073 10.8728 8.4539 13.6191 90 98.521 90
ZERR 2 0.0017 0.0011 0.0018 0 0.004 0
LATT 1
SYMM -X,0.5+Y,-Z
SFAC C H Cd I N
UNIT 32 48 2 8 4
DFIX 1.5 C9 C10 C10 C11 C1 C2 C2 C3
DFIX 1.47 N1 C1 N2 C9
DFIX 2.52 N1 C2 C1 C3 N2 C10 C9 C11
SIMU 0.02 0.04 1.6 N1 > C16
L.S. 20
PLAN 5
BOND
fmap 2
acta
OMIT -3 52
REM
REM
REM
WGHT 0.086200 8.810500
FVAR 0.13876
I1 4 0.290899 0.250000 0.661172 10.50000 0.06346 0.14487 =
0.05505 0.00000 0.00074 0.00000
I2 4 0.331934 -0.013562 0.381635 11.00000 0.08091 0.06036 =
0.08819 -0.01027 0.00787 0.00441
CD1 3 0.227170 0.250000 0.457676 10.50000 0.05907 0.06666 =
0.05908 0.00000 0.00608 0.00000
PART -1
I3 4 -0.029833 0.218326 0.402138 10.50000 0.05552 0.11924 =
0.06022 -0.01438 0.00131 0.00618
N1 5 -0.044351 0.275974 0.661668 10.50000 0.06982 0.10422 =
0.05470 0.00497 -0.00264 0.01035
AFIX 137
H1A 2 0.019702 0.310021 0.633660 10.50000 -1.20000
H1B 2 -0.112567 0.328919 0.636579 10.50000 -1.20000
H1C 2 -0.055862 0.173185 0.649500 10.50000 -1.20000
AFIX 0
C1 1 -0.018613 0.301917 0.768841 10.50000 0.05170 0.10466 =
0.06057 0.00539 0.01377 0.00792
AFIX 23
H1D 2 -0.091410 0.350496 0.789556 10.50000 -1.20000
H1E 2 0.049031 0.377382 0.781949 10.50000 -1.20000
AFIX 0
C2 1 0.014673 0.159890 0.832348 10.50000 0.04607 0.10600 =
0.07203 0.01359 0.02116 0.01068
AFIX 23
H2A 2 0.071022 0.094293 0.801126 10.50000 -1.20000
H2B 2 -0.060164 0.098766 0.835412 10.50000 -1.20000
AFIX 66 1.3900
C3 1 0.074177 0.197157 0.935801 10.50000 0.04947 0.09383 =
0.06908 0.00604 0.02217 0.00585
C4 1 0.186840 0.276647 0.957491 10.50000 0.06152 0.10642 =
0.08402 -0.00278 0.01176 0.00055
AFIX 43
H4 2 0.232114 0.301905 0.906816 10.50000 -1.20000
AFIX 65 1.3900
C5 1 0.231833 0.318384 1.054920 10.50000 0.08156 0.10426 =
0.09733 -0.01148 -0.01038 0.00391
AFIX 43
H5 2 0.307211 0.371567 1.069431 10.50000 -1.20000
AFIX 65 1.3900
C6 1 0.164165 0.280633 1.130661 10.50000 0.11083 0.09659 =
0.07767 -0.00219 -0.00606 0.01305
AFIX 43
H6 2 0.194268 0.308558 1.195847 10.50000 -1.20000
AFIX 65 1.3900
C7 1 0.051502 0.201143 1.108973 10.50000 0.10846 0.09154 =
0.06899 -0.00134 0.02889 0.01271
AFIX 43
H7 2 0.006228 0.175885 1.159648 10.50000 -1.20000
AFIX 65 1.3900
C8 1 0.006507 0.159404 1.011544 10.50000 0.07878 0.09404 =
0.07751 0.01030 0.02500 0.00777
AFIX 43
H8 2 -0.068871 0.106221 0.997033 10.50000 -1.20000
AFIX 0
N2 5 0.607099 0.235370 0.374810 10.50000 0.06922 0.11968 =
0.06874 -0.01498 0.01934 0.01533
AFIX 137
H2C 2 0.668589 0.165105 0.385420 10.50000 -1.20000
H2D 2 0.537959 0.193083 0.391159 10.50000 -1.20000
H2E 2 0.627410 0.320957 0.411723 10.50000 -1.20000
AFIX 0
C9 1 0.586254 0.279762 0.269667 10.50000 0.09976 0.12764 =
0.08100 -0.00712 0.00432 0.03335
AFIX 23
H9A 2 0.611414 0.389178 0.264571 10.50000 -1.20000
H9B 2 0.497598 0.274580 0.246420 10.50000 -1.20000
AFIX 0
C10 1 0.651546 0.183013 0.200512 10.50000 0.10419 0.12923 =
0.08379 -0.00245 0.01423 0.04213
AFIX 23
H10A 2 0.617867 0.076578 0.195714 10.50000 -1.20000
H10B 2 0.739524 0.176382 0.226116 10.50000 -1.20000
AFIX 66 1.3900
C11 1 0.633554 0.260620 0.097208 10.50000 0.09401 0.12808 =
0.07810 0.00156 0.01005 0.01406
C12 1 0.712402 0.159311 0.055676 10.50000 0.09547 0.12405 =
0.10708 0.01530 0.01073 0.00122
AFIX 43
H12 2 0.774447 0.104685 0.096386 10.50000 -1.20000
AFIX 65 1.3900
C13 1 0.698517 0.139647 -0.046703 10.50000 0.10982 0.09790 =
0.11293 0.00972 0.02197 0.00019
AFIX 43
H13 2 0.751271 0.071865 -0.074490 10.50000 -1.20000
AFIX 65 1.3900
C14 1 0.605783 0.221292 -0.107549 10.50000 0.08964 0.07727 =
0.09173 0.00726 0.02163 -0.00837
AFIX 43
H14 2 0.596493 0.208135 -0.176047 10.50000 -1.20000
AFIX 65 1.3900
C15 1 0.526934 0.322601 -0.066018 10.50000 0.09177 0.08360 =
0.09196 0.01103 0.01903 -0.00330
AFIX 43
H15 2 0.464890 0.377227 -0.106729 10.50000 -1.20000
AFIX 65 1.3900
C16 1 0.540818 0.342267 0.036360 10.50000 0.09335 0.10110 =
0.08674 -0.00133 0.01676 0.01155
AFIX 43
H16 2 0.488063 0.410049 0.064147 10.50000 -1.20000
AFIX 0
HKLF 4
REM z in P2(1)/m
REM R1 = 0.0704 for 2101 Fo > 4sig(Fo) and 0.0820 for all 2538 data
REM 171 parameters refined using 118 restraints
END
WGHT 0.0862 8.8153
REM Highest difference peak 1.145, deepest hole -2.148, 1-sigma level 0.322
Q1 1 0.4950 0.2500 0.5242 10.50000 0.05 1.14
Q2 1 0.1561 0.2500 1.2871 10.50000 0.05 0.98
Q3 1 0.4123 -0.0396 0.4894 11.00000 0.05 0.91
Q4 1 0.4192 0.0456 0.4621 11.00000 0.05 0.84
Q5 1 0.1582 0.2500 0.3438 10.50000 0.05 0.84
;
_shelx_res_checksum 81460
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_z
_database_code_depnum_ccdc_archive 'CCDC 1538297'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-05-04 downloaded from the CCDC.
;
_audit_creation_date 2017-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'Cd I4, 2(C8 H12 N)'
_chemical_formula_sum 'C16 H24 Cd I4 N2'
_chemical_formula_weight 864.37
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 4
_space_group_name_H-M_alt 'P 1 21 1'
_space_group_name_Hall 'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a 10.7635(12)
_cell_length_b 8.4013(8)
_cell_length_c 13.5791(13)
_cell_angle_alpha 90
_cell_angle_beta 98.698(3)
_cell_angle_gamma 90
_cell_volume 1213.8(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9900
_cell_measurement_temperature 220(2)
_cell_measurement_theta_max 27.515
_cell_measurement_theta_min 3.035
_shelx_estimated_absorpt_T_max 1.000
_shelx_estimated_absorpt_T_min 0.161
_exptl_absorpt_coefficient_mu 5.988
_exptl_absorpt_correction_T_max 1.000000
_exptl_absorpt_correction_T_min 0.160778
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ABSCOR
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 2.365
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 788
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max 1.000000
_exptl_transmission_factor_min 0.160778
_diffrn_reflns_av_R_equivalents 0.0595
_diffrn_reflns_av_unetI/netI 0.0714
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 9074
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.999
_diffrn_reflns_theta_min 3.035
_diffrn_ambient_temperature 220(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'multiwire proportional'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.869
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 1.000
_reflns_number_gt 4203
_reflns_number_total 4509
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.498
_refine_diff_density_min -0.841
_refine_diff_density_rms 0.201
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.52(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 197
_refine_ls_number_reflns 4509
_refine_ls_number_restraints 5
_refine_ls_R_factor_all 0.0453
_refine_ls_R_factor_gt 0.0415
_refine_ls_restrained_S_all 1.058
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.7820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1022
_refine_ls_wR_factor_ref 0.1076
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.48(7)
0.52(7)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
C1-C2 = C2-C3 = C10-C11
1.52 with sigma of 0.02
C9-C10
1.51 with sigma of 0.01
4. Others
Sof(I4')=1-FVAR(1)
Sof(I4)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
C1(H1D,H1E), C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16)
5.c Fitted hexagon refined as free rotating group:
C3(C4,C5,C6,C7,C8), C11(C12,C13,C14,C15,C16)
5.d Idealised Me refined as rotating group:
N1(H1A,H1B,H1C), N2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.70911(7) 0.2998(2) -0.16128(5) 0.0585(3) Uani 1 1 d . . . . .
I2 I 0.66057(10) 0.5427(2) 0.12364(7) 0.0494(2) Uani 1 1 d . . . . .
I3 I 0.67199(9) 0.0131(2) 0.11460(6) 0.0493(2) Uani 1 1 d . . . . .
I4 I 1.0315(3) 0.3156(17) 0.1002(4) 0.0576(16) Uani 0.79(4) 1 d . . P A 1
I4' I 1.0332(17) 0.253(5) 0.0999(14) 0.056(4) Uani 0.21(4) 1 d . . P A 2
Cd1 Cd 0.77156(7) 0.2857(2) 0.04323(5) 0.0419(2) Uani 1 1 d . . . . .
N1 N 1.0470(10) 0.2731(19) 0.8377(6) 0.060(3) Uani 1 1 d . . . . .
H1A H 1.090860 0.363053 0.846666 0.072 Uiso 1 1 calc GR . . . .
H1B H 1.091915 0.193631 0.868410 0.072 Uiso 1 1 calc GR . . . .
H1C H 0.975752 0.283613 0.862955 0.072 Uiso 1 1 calc GR . . . .
C1 C 1.0174(13) 0.2377(15) 0.7290(8) 0.054(3) Uani 1 1 d D . . . .
H1D H 0.949966 0.160238 0.717431 0.064 Uiso 1 1 calc R . . . .
H1E H 1.090772 0.192765 0.705823 0.064 Uiso 1 1 calc R . . . .
C2 C 0.9780(14) 0.3902(15) 0.6714(8) 0.052(3) Uani 1 1 d D . . . .
H2A H 1.050048 0.459761 0.671969 0.062 Uiso 1 1 calc R . . . .
H2B H 0.915115 0.446047 0.702348 0.062 Uiso 1 1 calc R . . . .
C3 C 0.9241(7) 0.3460(11) 0.5640(4) 0.046(3) Uani 1 1 d D . . . .
C4 C 0.9908(7) 0.3841(11) 0.4872(6) 0.055(3) Uani 1 1 d G . . . .
H4 H 1.067358 0.437055 0.501173 0.066 Uiso 1 1 calc R . . . .
C5 C 0.9432(10) 0.3431(13) 0.3897(5) 0.076(5) Uani 1 1 d G . . . .
H5 H 0.987849 0.368658 0.338285 0.091 Uiso 1 1 calc R . . . .
C6 C 0.8288(10) 0.2640(14) 0.3688(4) 0.072(4) Uani 1 1 d G . . . .
H6 H 0.796952 0.236585 0.303540 0.087 Uiso 1 1 calc R . . . .
C7 C 0.7621(8) 0.2259(13) 0.4456(6) 0.080(5) Uani 1 1 d G . . . .
H7 H 0.685563 0.172909 0.431683 0.097 Uiso 1 1 calc R . . . .
C8 C 0.8097(7) 0.2668(12) 0.5432(5) 0.055(3) Uani 1 1 d G . . . .
H8 H 0.765070 0.241304 0.594571 0.066 Uiso 1 1 calc R . . . .
N2 N 0.3908(10) 0.2747(19) 0.1282(6) 0.060(3) Uani 1 1 d . . . . .
H2C H 0.419545 0.192107 0.097251 0.072 Uiso 1 1 calc GR . . . .
H2D H 0.432064 0.362266 0.115367 0.072 Uiso 1 1 calc GR . . . .
H2E H 0.309173 0.287334 0.106497 0.072 Uiso 1 1 calc GR . . . .
C9 C 0.4104(15) 0.2451(15) 0.2374(8) 0.062(4) Uani 1 1 d D . . . .
H9A H 0.499869 0.236917 0.260786 0.075 Uiso 1 1 calc R . . . .
H9B H 0.372482 0.143781 0.249955 0.075 Uiso 1 1 calc R . . . .
C11 C 0.3664(9) 0.3290(11) 0.4047(4) 0.056(3) Uani 1 1 d D . . . .
C12 C 0.4604(8) 0.4007(11) 0.4715(6) 0.067(4) Uani 1 1 d G . . . .
H12 H 0.517687 0.468828 0.448248 0.080 Uiso 1 1 calc R . . . .
C13 C 0.4689(9) 0.3708(13) 0.5729(6) 0.073(5) Uani 1 1 d G . . . .
H13 H 0.531769 0.418823 0.617601 0.087 Uiso 1 1 calc R . . . .
C14 C 0.3833(11) 0.2690(13) 0.6076(5) 0.065(4) Uani 1 1 d G . . . .
H14 H 0.388960 0.248990 0.675507 0.078 Uiso 1 1 calc R . . . .
C15 C 0.2893(10) 0.1972(12) 0.5408(8) 0.086(5) Uani 1 1 d G . . . .
H15 H 0.232069 0.129159 0.564062 0.103 Uiso 1 1 calc R . . . .
C16 C 0.2809(8) 0.2272(12) 0.4394(7) 0.074(5) Uani 1 1 d G . . . .
H16 H 0.217985 0.179161 0.394709 0.088 Uiso 1 1 calc R . . . .
C10 C 0.3567(19) 0.3709(19) 0.2958(9) 0.083(6) Uani 1 1 d D . . . .
H10A H 0.269041 0.386864 0.268357 0.100 Uiso 1 1 calc R . . . .
H10B H 0.400773 0.470137 0.289249 0.100 Uiso 1 1 calc 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
I1 0.0427(4) 0.0957(7) 0.0348(3) -0.0006(5) -0.0012(3) 0.0074(5)
I2 0.0503(6) 0.0406(5) 0.0561(5) -0.0079(3) 0.0039(4) 0.0000(3)
I3 0.0534(6) 0.0398(5) 0.0532(5) 0.0031(3) 0.0033(4) -0.0031(3)
I4 0.0340(10) 0.097(4) 0.0402(9) -0.0132(17) 0.0004(6) 0.0002(15)
I4' 0.054(5) 0.075(10) 0.036(4) 0.004(5) 0.001(3) -0.009(5)
Cd1 0.0412(4) 0.0456(4) 0.0377(4) 0.0006(4) 0.0020(3) -0.0013(4)
N1 0.046(6) 0.097(8) 0.035(4) 0.000(6) -0.004(4) 0.019(7)
C1 0.052(8) 0.079(9) 0.029(5) -0.004(5) 0.002(5) 0.010(6)
C2 0.054(8) 0.062(7) 0.039(6) -0.005(5) 0.003(5) -0.001(6)
C3 0.051(7) 0.054(6) 0.033(5) -0.002(4) 0.003(5) 0.010(5)
C4 0.067(10) 0.055(7) 0.043(7) -0.001(5) 0.012(6) 0.003(6)
C5 0.128(16) 0.072(9) 0.034(6) 0.013(6) 0.031(8) 0.022(9)
C6 0.093(12) 0.073(9) 0.043(6) -0.013(7) -0.013(7) 0.018(9)
C7 0.061(10) 0.095(12) 0.072(10) -0.009(8) -0.034(8) -0.001(8)
C8 0.054(7) 0.068(8) 0.040(5) 0.001(6) -0.001(5) -0.005(7)
N2 0.045(6) 0.089(7) 0.043(5) -0.011(6) 0.001(4) -0.007(7)
C9 0.084(11) 0.069(10) 0.035(6) 0.009(5) 0.014(6) 0.004(7)
C11 0.051(7) 0.073(9) 0.039(6) -0.019(5) -0.005(5) 0.021(6)
C12 0.053(9) 0.065(8) 0.082(11) -0.009(7) 0.009(7) -0.013(7)
C13 0.083(12) 0.078(10) 0.050(8) -0.021(7) -0.015(7) 0.014(8)
C14 0.086(10) 0.072(8) 0.041(6) 0.008(7) 0.024(6) 0.023(9)
C15 0.080(13) 0.064(10) 0.124(16) 0.011(9) 0.050(12) 0.004(9)
C16 0.051(9) 0.102(12) 0.072(10) -0.022(8) 0.020(7) -0.020(8)
C10 0.101(14) 0.103(13) 0.044(8) 0.016(7) 0.006(8) 0.048(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Cd1 2.7593(10) . ?
I2 Cd1 2.7710(11) . ?
I3 Cd1 2.7654(12) . ?
I4 Cd1 2.799(4) . ?
I4' Cd1 2.819(19) . ?
N1 C1 1.492(13) . ?
C1 C2 1.528(15) . ?
C2 C3 1.531(12) . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
N2 C9 1.487(14) . ?
C9 C10 1.489(11) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C11 C10 1.509(13) . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Cd1 I2 108.00(4) . . ?
I1 Cd1 I3 109.88(4) . . ?
I1 Cd1 I4 110.82(12) . . ?
I1 Cd1 I4' 111.1(4) . . ?
I2 Cd1 I4 107.1(2) . . ?
I2 Cd1 I4' 116.2(9) . . ?
I3 Cd1 I2 107.12(3) . . ?
I3 Cd1 I4 113.7(3) . . ?
I3 Cd1 I4' 104.3(6) . . ?
N1 C1 C2 109.9(10) . . ?
C1 C2 C3 108.7(9) . . ?
C4 C3 C2 119.6(7) . . ?
C4 C3 C8 120.0 . . ?
C8 C3 C2 120.4(7) . . ?
C5 C4 C3 120.0 . . ?
C4 C5 C6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C7 C8 C3 120.0 . . ?
N2 C9 C10 113.9(11) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C10 118.3(11) . . ?
C16 C11 C10 121.6(11) . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
C9 C10 C11 112.4(10) . . ?
_shelx_res_file
;
TITL z in P2(1)
z.res
created by SHELXL-2016/6 at 09:54:51 on 06-Mar-2017
CELL 0.71073 10.7635 8.4013 13.5791 90 98.698 90
ZERR 2 0.0012 0.0008 0.0013 0 0.003 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC C H Cd I N
UNIT 32 48 2 8 4
DFIX 1.52 C1 C2 C2 C3 C10 C11
DFIX 1.51 0.01 C9 C10
L.S. 50
PLAN 2
BOND
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT -3 52
OMIT -10 0 6
OMIT -3 -5 10
REM
REM
REM
WGHT 0.057000 0.782000
BASF 0.52000
FVAR 0.18009 0.78893
I1 4 0.709112 0.299850 -0.161279 11.00000 0.04275 0.09568 =
0.03481 -0.00057 -0.00116 0.00740
I2 4 0.660566 0.542737 0.123643 11.00000 0.05033 0.04058 =
0.05608 -0.00785 0.00394 -0.00003
I3 4 0.671988 0.013053 0.114602 11.00000 0.05343 0.03983 =
0.05325 0.00307 0.00334 -0.00310
PART 1
I4 4 1.031466 0.315587 0.100177 21.00000 0.03399 0.09700 =
0.04018 -0.01320 0.00036 0.00017
PART 0
PART 2
I4' 4 1.033223 0.252734 0.099917 -21.00000 0.05449 0.07534 =
0.03587 0.00418 0.00106 -0.00875
PART 0
CD1 3 0.771561 0.285671 0.043234 11.00000 0.04123 0.04561 =
0.03769 0.00063 0.00203 -0.00128
N1 5 1.046964 0.273070 0.837730 11.00000 0.04580 0.09680 =
0.03467 -0.00027 -0.00361 0.01900
AFIX 137
H1A 2 1.090860 0.363053 0.846666 11.00000 -1.20000
H1B 2 1.091915 0.193631 0.868410 11.00000 -1.20000
H1C 2 0.975752 0.283613 0.862955 11.00000 -1.20000
AFIX 0
C1 1 1.017404 0.237723 0.729034 11.00000 0.05218 0.07867 =
0.02882 -0.00406 0.00160 0.00978
AFIX 23
H1D 2 0.949966 0.160238 0.717431 11.00000 -1.20000
H1E 2 1.090772 0.192765 0.705823 11.00000 -1.20000
AFIX 0
C2 1 0.978000 0.390222 0.671390 11.00000 0.05354 0.06235 =
0.03893 -0.00457 0.00306 -0.00053
AFIX 23
H2A 2 1.050048 0.459761 0.671969 11.00000 -1.20000
H2B 2 0.915115 0.446047 0.702348 11.00000 -1.20000
AFIX 66 1.3900
C3 1 0.924098 0.345962 0.564022 11.00000 0.05061 0.05389 =
0.03327 -0.00223 0.00298 0.01024
C4 1 0.990835 0.384112 0.487245 11.00000 0.06719 0.05489 =
0.04293 -0.00137 0.01199 0.00257
AFIX 43
H4 2 1.067358 0.437055 0.501173 11.00000 -1.20000
AFIX 65 1.3900
C5 1 0.943198 0.343132 0.389653 11.00000 0.12763 0.07177 =
0.03368 0.01329 0.03054 0.02243
AFIX 43
H5 2 0.987849 0.368658 0.338285 11.00000 -1.20000
AFIX 65 1.3900
C6 1 0.828824 0.264002 0.368836 11.00000 0.09304 0.07324 =
0.04331 -0.01257 -0.01312 0.01802
AFIX 43
H6 2 0.796952 0.236585 0.303540 11.00000 -1.20000
AFIX 65 1.3900
C7 1 0.762086 0.225851 0.445611 11.00000 0.06054 0.09534 =
0.07179 -0.00931 -0.03425 -0.00089
AFIX 43
H7 2 0.685563 0.172909 0.431683 11.00000 -1.20000
AFIX 65 1.3900
C8 1 0.809722 0.266830 0.543204 11.00000 0.05374 0.06826 =
0.04024 0.00115 -0.00050 -0.00515
AFIX 43
H8 2 0.765070 0.241304 0.594571 11.00000 -1.20000
AFIX 0
N2 5 0.390827 0.274670 0.128161 11.00000 0.04473 0.08927 =
0.04320 -0.01124 0.00098 -0.00676
AFIX 137
H2C 2 0.419545 0.192107 0.097251 11.00000 -1.20000
H2D 2 0.432064 0.362266 0.115367 11.00000 -1.20000
H2E 2 0.309173 0.287334 0.106497 11.00000 -1.20000
AFIX 0
C9 1 0.410376 0.245094 0.237403 11.00000 0.08446 0.06923 =
0.03471 0.00934 0.01396 0.00438
AFIX 23
H9A 2 0.499869 0.236917 0.260786 11.00000 -1.20000
H9B 2 0.372482 0.143781 0.249955 11.00000 -1.20000
AFIX 66 1.3900
C11 1 0.366441 0.328953 0.404688 11.00000 0.05122 0.07281 =
0.03910 -0.01941 -0.00534 0.02084
C12 1 0.460440 0.400748 0.471460 11.00000 0.05331 0.06473 =
0.08223 -0.00876 0.00890 -0.01341
AFIX 43
H12 2 0.517687 0.468828 0.448248 11.00000 -1.20000
AFIX 65 1.3900
C13 1 0.468877 0.370788 0.572926 11.00000 0.08261 0.07831 =
0.04958 -0.02075 -0.01486 0.01388
AFIX 43
H13 2 0.531769 0.418823 0.617601 11.00000 -1.20000
AFIX 65 1.3900
C14 1 0.383315 0.269034 0.607620 11.00000 0.08613 0.07182 =
0.04141 0.00811 0.02366 0.02344
AFIX 43
H14 2 0.388960 0.248990 0.675507 11.00000 -1.20000
AFIX 65 1.3900
C15 1 0.289315 0.197239 0.540849 11.00000 0.08045 0.06419 =
0.12361 0.01054 0.04991 0.00448
AFIX 43
H15 2 0.232069 0.129159 0.564062 11.00000 -1.20000
AFIX 65 1.3900
C16 1 0.280877 0.227197 0.439383 11.00000 0.05054 0.10159 =
0.07233 -0.02243 0.02042 -0.01990
AFIX 43
H16 2 0.217985 0.179161 0.394709 11.00000 -1.20000
AFIX 0
C10 1 0.356720 0.370863 0.295751 11.00000 0.10061 0.10307 =
0.04387 0.01579 0.00612 0.04798
AFIX 23
H10A 2 0.269041 0.386864 0.268357 11.00000 -1.20000
H10B 2 0.400773 0.470137 0.289249 11.00000 -1.20000
AFIX 0
HKLF 4
REM z in P2(1)
REM R1 = 0.0415 for 4203 Fo > 4sig(Fo) and 0.0453 for all 4509 data
REM 197 parameters refined using 5 restraints
END
WGHT 0.0569 0.8175
REM Highest difference peak 1.498, deepest hole -0.841, 1-sigma level 0.201
Q1 1 0.7572 0.2134 -0.1590 11.00000 0.05 1.50
Q2 1 0.7575 0.3815 -0.1585 11.00000 0.05 1.34
;
_shelx_res_checksum 36528
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.48(7)
2 0.52(7)