# Electronic Supplementary Material (ESI) for Soft Matter
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_name_full 'Soft Matter'
_journal_coden_cambridge 0777
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_author_name P.Dastidar
_publ_contact_author_name 'Parthasarathi Dastidar'
_publ_contact_author_email parthod123@rediffmail.com
data_pdann
_database_code_depnum_ccdc_archive 'CCDC 870562'
#TrackingRef 'CP1-R1.cif'
_audit_update_record
;
2012-05-21 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C30 H46 Cd N3 O23'
_chemical_formula_weight 929.10
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 17.9224(13)
_cell_length_b 26.390(2)
_cell_length_c 9.0841(7)
_cell_angle_alpha 90.00
_cell_angle_beta 99.700(2)
_cell_angle_gamma 90.00
_cell_volume 4235.1(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 298(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description plate
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.457
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1916
_exptl_absorpt_coefficient_mu 0.601
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8310
_exptl_absorpt_correction_T_max 0.9206
_exptl_absorpt_process_details sadabs
_exptl_special_details ?
_diffrn_ambient_temperature 298(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Apex II'
_diffrn_measurement_method 'omega scan'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 23677
_diffrn_reflns_av_R_equivalents 0.0656
_diffrn_reflns_av_sigmaI/netI 0.0400
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_theta_min 1.15
_diffrn_reflns_theta_max 19.75
_reflns_number_total 3803
_reflns_number_gt 3109
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker Apex II'
_computing_cell_refinement 'Bruker Apex II'
_computing_data_reduction SAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Mercury 2.3'
_computing_publication_material Shelxl-97
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3803
_refine_ls_number_parameters 406
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0636
_refine_ls_R_factor_gt 0.0437
_refine_ls_wR_factor_ref 0.1023
_refine_ls_wR_factor_gt 0.0934
_refine_ls_goodness_of_fit_ref 1.107
_refine_ls_restrained_S_all 1.107
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd -0.08129(2) 1.076403(16) -0.47420(5) 0.0594(2) Uani 1 1 d . . .
O1 O -0.0177(2) 1.01865(16) -0.3106(4) 0.0683(12) Uani 1 1 d . . .
O2 O 0.0203(3) 1.0959(2) -0.2602(5) 0.0930(16) Uani 1 1 d . . .
C3 C 0.0239(4) 1.0491(3) -0.2296(7) 0.0656(18) Uani 1 1 d . . .
C4 C 0.0795(3) 1.0331(3) -0.0965(7) 0.0546(16) Uani 1 1 d . . .
C5 C 0.0838(3) 0.9822(3) -0.0562(6) 0.0606(18) Uani 1 1 d . . .
H5 H 0.0526 0.9587 -0.1126 0.073 Uiso 1 1 calc R . .
C6 C 0.1348(3) 0.9663(2) 0.0683(6) 0.0626(18) Uani 1 1 d . . .
H6 H 0.1365 0.9324 0.0966 0.075 Uiso 1 1 calc R . .
C7 C 0.1829(3) 1.0011(3) 0.1498(6) 0.0549(16) Uani 1 1 d . . .
C8 C 0.1776(4) 1.0513(3) 0.1101(7) 0.076(2) Uani 1 1 d . . .
H8 H 0.2090 1.0753 0.1643 0.091 Uiso 1 1 calc R . .
C9 C 0.1255(4) 1.0656(2) -0.0105(8) 0.078(2) Uani 1 1 d . . .
H9 H 0.1217 1.0999 -0.0346 0.094 Uiso 1 1 calc R . .
N10 N 0.2346(3) 0.98102(18) 0.2708(5) 0.0551(13) Uani 1 1 d . . .
H10 H 0.2292 0.9494 0.2898 0.066 Uiso 1 1 calc R . .
C11 C 0.2905(3) 1.0048(3) 0.3588(7) 0.0601(17) Uani 1 1 d . . .
O12 O 0.3032(3) 1.0493(2) 0.3496(5) 0.0946(17) Uani 1 1 d . . .
C13 C 0.3416(3) 0.9725(3) 0.4743(6) 0.0559(16) Uani 1 1 d . . .
C14 C 0.3268(3) 0.9227(2) 0.5030(6) 0.0567(16) Uani 1 1 d . . .
H14 H 0.2847 0.9069 0.4482 0.068 Uiso 1 1 calc R . .
C15 C 0.3741(3) 0.8958(3) 0.6135(7) 0.0608(17) Uani 1 1 d . . .
C16 C 0.4353(3) 0.9211(3) 0.6964(6) 0.0665(18) Uani 1 1 d . . .
H16 H 0.4674 0.9036 0.7704 0.080 Uiso 1 1 calc R . .
C17 C 0.4494(3) 0.9710(3) 0.6718(6) 0.0497(16) Uani 1 1 d . . .
C18 C 0.4025(3) 0.9967(2) 0.5605(6) 0.0557(17) Uani 1 1 d . . .
H18 H 0.4118 1.0307 0.5431 0.067 Uiso 1 1 calc R . .
C19 C 0.5123(3) 1.0009(3) 0.7670(7) 0.0644(19) Uani 1 1 d . . .
O20 O 0.5147(3) 1.0467(2) 0.7527(5) 0.0969(17) Uani 1 1 d . . .
N21 N 0.5605(3) 0.97450(19) 0.8662(5) 0.0645(15) Uani 1 1 d . . .
H21 H 0.5538 0.9422 0.8646 0.077 Uiso 1 1 calc R . .
C22 C 0.6203(3) 0.9923(3) 0.9721(7) 0.0594(17) Uani 1 1 d . . .
C23 C 0.6548(4) 0.9596(2) 1.0773(7) 0.0695(19) Uani 1 1 d . . .
H23 H 0.6371 0.9265 1.0768 0.083 Uiso 1 1 calc R . .
C24 C 0.7148(3) 0.9737(3) 1.1849(7) 0.0659(19) Uani 1 1 d . . .
H24 H 0.7378 0.9497 1.2530 0.079 Uiso 1 1 calc R . .
C25 C 0.7414(3) 1.0227(3) 1.1929(6) 0.0495(15) Uani 1 1 d . . .
C26 C 0.8045(3) 1.0395(3) 1.3096(7) 0.0567(17) Uani 1 1 d . . .
O27 O 0.8383(2) 1.00890(15) 1.4040(4) 0.0661(12) Uani 1 1 d . . .
O28 O 0.8233(2) 1.08497(17) 1.3154(4) 0.0664(12) Uani 1 1 d . . .
C29 C 0.7083(3) 1.0566(2) 1.0865(6) 0.0583(17) Uani 1 1 d . . .
H29 H 0.7265 1.0897 1.0872 0.070 Uiso 1 1 calc R . .
C30 C 0.6469(3) 1.0417(3) 0.9762(7) 0.0653(18) Uani 1 1 d . . .
H30 H 0.6243 1.0651 0.9060 0.078 Uiso 1 1 calc R . .
C31 C 0.3556(4) 0.8434(3) 0.6544(8) 0.076(2) Uani 1 1 d . . .
O32 O 0.4054(3) 0.8112(2) 0.6769(7) 0.128(2) Uani 1 1 d . . .
N33 N 0.2837(3) 0.83454(19) 0.6694(5) 0.0639(14) Uani 1 1 d . . .
H33 H 0.2526 0.8593 0.6476 0.077 Uiso 1 1 calc R . .
C34 C 0.2528(4) 0.7888(3) 0.7174(7) 0.0608(18) Uani 1 1 d . . .
C35 C 0.2785(4) 0.7416(3) 0.6909(8) 0.082(2) Uani 1 1 d . . .
H35 H 0.3195 0.7376 0.6413 0.098 Uiso 1 1 calc R . .
C36 C 0.2429(4) 0.7002(3) 0.7389(8) 0.0723(19) Uani 1 1 d . . .
H36 H 0.2600 0.6680 0.7197 0.087 Uiso 1 1 calc R . .
C37 C 0.1830(4) 0.7047(3) 0.8140(7) 0.0620(18) Uani 1 1 d . . .
C38 C 0.1462(4) 0.6589(3) 0.8682(7) 0.0595(18) Uani 1 1 d . . .
O39 O 0.1660(2) 0.61546(16) 0.8356(4) 0.0619(12) Uani 1 1 d . . .
O40 O 0.0951(3) 0.66482(15) 0.9474(5) 0.0688(13) Uani 1 1 d . . .
C41 C 0.1593(4) 0.7525(3) 0.8380(8) 0.076(2) Uani 1 1 d . . .
H41 H 0.1189 0.7567 0.8892 0.091 Uiso 1 1 calc R . .
C42 C 0.1927(4) 0.7945(3) 0.7895(8) 0.076(2) Uani 1 1 d . . .
H42 H 0.1745 0.8267 0.8057 0.091 Uiso 1 1 calc R . .
O43 O 0.0114(2) 1.07738(15) -0.6201(4) 0.0771(12) Uani 1 1 d . . .
O44 O 0.8432(3) 0.9077(2) 0.4737(7) 0.137(2) Uani 1 1 d . . .
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
Cd1 0.0524(3) 0.0560(3) 0.0592(3) -0.0034(3) -0.0208(2) 0.0029(3)
O1 0.062(3) 0.078(3) 0.053(3) -0.005(2) -0.024(2) -0.001(2)
O2 0.096(4) 0.087(4) 0.078(3) 0.002(3) -0.037(3) 0.008(3)
C3 0.066(5) 0.068(5) 0.060(5) 0.011(5) 0.003(4) 0.014(4)
C4 0.045(4) 0.063(5) 0.049(4) 0.003(4) -0.012(4) 0.002(4)
C5 0.035(4) 0.090(6) 0.050(4) -0.012(4) -0.012(4) -0.009(4)
C6 0.056(4) 0.075(5) 0.050(4) 0.004(4) -0.012(4) -0.007(4)
C7 0.050(4) 0.076(5) 0.035(4) -0.007(4) -0.005(3) -0.008(4)
C8 0.090(5) 0.058(5) 0.062(5) 0.005(4) -0.036(4) -0.010(4)
C9 0.074(5) 0.065(5) 0.082(5) 0.006(4) -0.022(4) -0.003(4)
N10 0.047(3) 0.066(3) 0.043(3) 0.008(3) -0.017(3) -0.012(3)
C11 0.053(4) 0.073(5) 0.049(4) 0.003(4) -0.005(4) -0.008(4)
O12 0.096(4) 0.070(3) 0.095(4) 0.015(3) -0.051(3) -0.025(3)
C13 0.045(4) 0.073(5) 0.045(4) -0.005(4) -0.008(4) -0.003(4)
C14 0.050(4) 0.062(5) 0.053(4) -0.010(4) -0.007(3) -0.008(4)
C15 0.038(4) 0.075(5) 0.061(4) -0.003(4) -0.014(4) -0.002(4)
C16 0.045(4) 0.095(6) 0.052(4) 0.010(4) -0.013(3) -0.004(4)
C17 0.037(4) 0.061(5) 0.046(4) 0.001(3) -0.008(3) -0.008(3)
C18 0.038(4) 0.079(5) 0.047(4) 0.000(4) -0.003(4) -0.012(4)
C19 0.050(4) 0.087(6) 0.049(4) -0.007(4) -0.012(4) -0.012(5)
O20 0.088(4) 0.083(4) 0.096(4) 0.007(3) -0.053(3) -0.022(3)
N21 0.042(3) 0.078(4) 0.060(3) -0.003(3) -0.030(3) -0.008(3)
C22 0.047(4) 0.073(5) 0.052(4) -0.001(4) -0.008(4) 0.000(4)
C23 0.067(5) 0.053(4) 0.077(5) -0.005(4) -0.019(4) -0.005(4)
C24 0.047(4) 0.074(5) 0.067(5) 0.004(4) -0.018(4) 0.005(4)
C25 0.032(4) 0.067(5) 0.043(4) -0.002(4) -0.010(3) 0.004(4)
C26 0.049(4) 0.059(5) 0.058(5) -0.006(4) -0.003(4) 0.011(4)
O27 0.067(3) 0.063(3) 0.058(3) -0.006(2) -0.019(2) -0.002(2)
O28 0.061(3) 0.065(3) 0.062(3) -0.008(2) -0.020(2) 0.001(2)
C29 0.043(4) 0.078(5) 0.047(4) -0.013(4) -0.013(3) -0.007(3)
C30 0.048(4) 0.084(5) 0.056(4) 0.010(4) -0.012(4) 0.003(4)
C31 0.049(5) 0.059(5) 0.107(6) 0.010(4) -0.027(4) 0.004(4)
O32 0.058(3) 0.093(4) 0.222(7) 0.039(4) -0.004(4) 0.011(3)
N33 0.055(4) 0.056(4) 0.072(4) 0.007(3) -0.015(3) 0.004(3)
C34 0.050(5) 0.057(6) 0.065(5) 0.017(4) -0.017(4) -0.010(4)
C35 0.090(6) 0.049(5) 0.105(6) 0.006(4) 0.010(4) 0.002(5)
C36 0.081(5) 0.050(5) 0.085(5) -0.003(4) 0.011(5) 0.010(4)
C37 0.067(5) 0.055(6) 0.056(4) 0.002(4) -0.012(4) 0.007(4)
C38 0.059(5) 0.056(5) 0.053(5) 0.009(4) -0.022(4) -0.012(5)
O39 0.062(3) 0.043(3) 0.071(3) -0.002(2) -0.016(2) 0.002(2)
O40 0.073(3) 0.052(3) 0.078(3) 0.008(2) 0.003(3) -0.001(2)
C41 0.071(5) 0.058(5) 0.098(6) 0.009(4) 0.011(4) 0.007(5)
C42 0.071(5) 0.062(6) 0.092(6) 0.008(4) 0.009(5) 0.003(4)
O43 0.074(3) 0.083(3) 0.069(3) 0.001(2) -0.004(2) 0.003(2)
O44 0.098(4) 0.122(4) 0.167(5) 0.035(4) -0.046(4) -0.017(3)
_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
Cd1 O1 2.293(4) . ?
Cd1 O43 2.294(4) . ?
Cd1 O28 2.351(4) 1_453 ?
Cd1 O40 2.363(4) 2 ?
Cd1 O39 2.366(4) 2 ?
Cd1 O27 2.437(4) 1_453 ?
Cd1 O2 2.483(4) . ?
Cd1 C38 2.720(7) 2 ?
Cd1 C3 2.757(7) . ?
O1 C3 1.249(7) . ?
O2 C3 1.265(7) . ?
C3 C4 1.493(8) . ?
C4 C9 1.346(8) . ?
C4 C5 1.389(8) . ?
C5 C6 1.393(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.386(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.373(7) . ?
C7 N10 1.416(7) . ?
C8 C9 1.367(8) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N10 C11 1.330(7) . ?
N10 H10 0.8600 . ?
C11 O12 1.201(7) . ?
C11 C13 1.532(8) . ?
C13 C14 1.372(7) . ?
C13 C18 1.387(7) . ?
C14 C15 1.395(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.393(8) . ?
C15 C31 1.482(8) . ?
C16 C17 1.365(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(7) . ?
C17 C19 1.521(8) . ?
C18 H18 0.9300 . ?
C19 O20 1.216(7) . ?
C19 N21 1.334(7) . ?
N21 C22 1.396(7) . ?
N21 H21 0.8600 . ?
C22 C23 1.357(7) . ?
C22 C30 1.385(8) . ?
C23 C24 1.377(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(8) . ?
C24 H24 0.9300 . ?
C25 C29 1.376(7) . ?
C25 C26 1.481(8) . ?
C26 O28 1.246(7) . ?
C26 O27 1.257(6) . ?
O27 Cd1 2.437(4) 1_657 ?
O28 Cd1 2.351(4) 1_657 ?
C29 C30 1.414(7) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O32 1.225(7) . ?
C31 N33 1.339(7) . ?
N33 C34 1.427(7) . ?
N33 H33 0.8600 . ?
C34 C42 1.360(8) . ?
C34 C35 1.363(8) . ?
C35 C36 1.374(8) . ?
C35 H35 0.9300 . ?
C36 C37 1.370(8) . ?
C36 H36 0.9300 . ?
C37 C41 1.360(8) . ?
C37 C38 1.499(8) . ?
C38 O39 1.251(7) . ?
C38 O40 1.267(7) . ?
C38 Cd1 2.720(7) 2_545 ?
O39 Cd1 2.367(4) 2_545 ?
O40 Cd1 2.363(4) 2_545 ?
C41 C42 1.369(8) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
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
O1 Cd1 O43 93.02(14) . . ?
O1 Cd1 O28 143.58(16) . 1_453 ?
O43 Cd1 O28 91.57(14) . 1_453 ?
O1 Cd1 O40 129.69(15) . 2 ?
O43 Cd1 O40 98.45(16) . 2 ?
O28 Cd1 O40 85.09(14) 1_453 2 ?
O1 Cd1 O39 103.78(14) . 2 ?
O43 Cd1 O39 153.52(15) . 2 ?
O28 Cd1 O39 86.94(13) 1_453 2 ?
O40 Cd1 O39 55.07(14) 2 2 ?
O1 Cd1 O27 89.98(16) . 1_453 ?
O43 Cd1 O27 100.14(14) . 1_453 ?
O28 Cd1 O27 53.67(13) 1_453 1_453 ?
O40 Cd1 O27 134.80(14) 2 1_453 ?
O39 Cd1 O27 100.18(13) 2 1_453 ?
O1 Cd1 O2 53.98(14) . . ?
O43 Cd1 O2 86.75(15) . . ?
O28 Cd1 O2 162.44(17) 1_453 . ?
O40 Cd1 O2 77.88(15) 2 . ?
O39 Cd1 O2 86.83(14) 2 . ?
O27 Cd1 O2 143.77(17) 1_453 . ?
O1 Cd1 C38 119.88(17) . 2 ?
O43 Cd1 C38 126.2(2) . 2 ?
O28 Cd1 C38 85.11(15) 1_453 2 ?
O40 Cd1 C38 27.73(16) 2 2 ?
O39 Cd1 C38 27.35(17) 2 2 ?
O27 Cd1 C38 119.37(18) 1_453 2 ?
O2 Cd1 C38 81.83(17) . 2 ?
O1 Cd1 C3 26.67(16) . . ?
O43 Cd1 C3 90.29(16) . . ?
O28 Cd1 C3 170.2(2) 1_453 . ?
O40 Cd1 C3 104.1(2) 2 . ?
O39 Cd1 C3 95.63(16) 2 . ?
O27 Cd1 C3 116.6(2) 1_453 . ?
O2 Cd1 C3 27.31(16) . . ?
C38 Cd1 C3 101.49(19) 2 . ?
C3 O1 Cd1 97.8(4) . . ?
C3 O2 Cd1 88.5(4) . . ?
O1 C3 O2 119.7(6) . . ?
O1 C3 C4 123.0(7) . . ?
O2 C3 C4 117.3(7) . . ?
O1 C3 Cd1 55.5(3) . . ?
O2 C3 Cd1 64.2(3) . . ?
C4 C3 Cd1 178.3(6) . . ?
C9 C4 C5 117.5(5) . . ?
C9 C4 C3 123.3(7) . . ?
C5 C4 C3 119.2(6) . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C8 C7 C6 119.4(6) . . ?
C8 C7 N10 124.9(5) . . ?
C6 C7 N10 115.7(6) . . ?
C9 C8 C7 119.0(6) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C4 C9 C8 123.9(6) . . ?
C4 C9 H9 118.0 . . ?
C8 C9 H9 118.0 . . ?
C11 N10 C7 128.2(5) . . ?
C11 N10 H10 115.9 . . ?
C7 N10 H10 115.9 . . ?
O12 C11 N10 123.5(6) . . ?
O12 C11 C13 119.7(6) . . ?
N10 C11 C13 116.8(6) . . ?
C14 C13 C18 119.5(5) . . ?
C14 C13 C11 123.4(6) . . ?
C18 C13 C11 116.9(6) . . ?
C13 C14 C15 120.7(5) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 118.1(6) . . ?
C16 C15 C31 120.1(6) . . ?
C14 C15 C31 121.4(6) . . ?
C17 C16 C15 121.7(6) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 119.2(5) . . ?
C16 C17 C19 123.2(6) . . ?
C18 C17 C19 117.6(6) . . ?
C17 C18 C13 120.7(6) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
O20 C19 N21 124.1(6) . . ?
O20 C19 C17 119.4(6) . . ?
N21 C19 C17 116.5(6) . . ?
C19 N21 C22 128.6(6) . . ?
C19 N21 H21 115.7 . . ?
C22 N21 H21 115.7 . . ?
C23 C22 C30 117.7(6) . . ?
C23 C22 N21 118.5(6) . . ?
C30 C22 N21 123.8(6) . . ?
C22 C23 C24 122.5(6) . . ?
C22 C23 H23 118.7 . . ?
C24 C23 H23 118.7 . . ?
C23 C24 C25 120.8(6) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C29 C25 C24 118.1(5) . . ?
C29 C25 C26 119.7(6) . . ?
C24 C25 C26 122.2(6) . . ?
O28 C26 O27 119.6(5) . . ?
O28 C26 C25 119.1(6) . . ?
O27 C26 C25 121.3(6) . . ?
C26 O27 Cd1 91.2(4) . 1_657 ?
C26 O28 Cd1 95.5(4) . 1_657 ?
C25 C29 C30 120.5(6) . . ?
C25 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C22 C30 C29 120.3(6) . . ?
C22 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
O32 C31 N33 123.2(6) . . ?
O32 C31 C15 120.1(7) . . ?
N33 C31 C15 116.7(6) . . ?
C31 N33 C34 127.6(6) . . ?
C31 N33 H33 116.2 . . ?
C34 N33 H33 116.2 . . ?
C42 C34 C35 120.4(6) . . ?
C42 C34 N33 115.7(7) . . ?
C35 C34 N33 123.9(7) . . ?
C34 C35 C36 118.8(7) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C37 C36 C35 122.2(6) . . ?
C37 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
C41 C37 C36 117.0(6) . . ?
C41 C37 C38 121.8(8) . . ?
C36 C37 C38 121.2(7) . . ?
O39 C38 O40 120.6(6) . . ?
O39 C38 C37 120.2(7) . . ?
O40 C38 C37 119.2(7) . . ?
O39 C38 Cd1 60.4(3) . 2_545 ?
O40 C38 Cd1 60.3(3) . 2_545 ?
C37 C38 Cd1 178.5(4) . 2_545 ?
C38 O39 Cd1 92.3(4) . 2_545 ?
C38 O40 Cd1 92.0(4) . 2_545 ?
C37 C41 C42 122.3(7) . . ?
C37 C41 H41 118.9 . . ?
C42 C41 H41 118.9 . . ?
C34 C42 C41 119.4(7) . . ?
C34 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N10 H10 O39 0.86 2.13 2.929(6) 154.1 4_575
N33 H33 O28 0.86 2.07 2.881(6) 157.1 3_677
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 19.75
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.324
_refine_diff_density_min -0.248
_vrf_CHEMW03_pdann
;
PROBLEM: The ratio of given/expected molecular weight as calculated from the
atom site data lies outside the range 0.90 <> 1.10
RESPONSE: We have used SQUEEZE to remove the contributions of disordered
solvent molecules (which we could not be modeled) within the crystal
lattice. Therefore, the contribution of disordered solvent molecules removed
by the SQUEEZE process are included in the overall formula, formula weight,
density, F(000) etc. The output of the PLATON (generated as. sqf
file) is also appended to the bottom of the CIF.
;
_vrf_THETM01_pdann
;
PROBLEM: The value of sine(theta_max)/wavelength is less that 0.550 Calculated
sin(theta_max)/wavelength = 0.4755
RESPONSE: The crystal was poorly diffracting at higher Bragg angles. The
situation did not improve even after repeating crystallization and fresh data
collection.
;
_vrf_PLAT043_pdann
;
PROBLEM: Check Reported Molecular Weight ...... 929.10
RESPONSE: We have used SQUEEZE to remove the contributions
of disordered solvent molecules (which we could not be modeled) within the
crystal lattice. Therefore, the contribution of disordered solvent molecules
removed by the SQUEEZE process are included in the overall formula,
formula weight, density, F(000) etc. The output of the PLATON (generated as .sqf file) is also
appended to the bottom of the CIF.
;
_vrf_PLAT306_pdann
;
PROBLEM: Isolated Oxygen Atom (H-atom Missing?) .... O44
RESPONSE: The hydrogen atoms of the lattice included water molecules could not
be located from differnce Fourier map.
;
_vrf_PLAT051_pdann
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by. 6.45 Perc.
RESPONSE: We have used SQUEEZE to remove the contributions of disordered
solvent molecules (which we could not be modeled) within the crystal lattice.
Therefore, the contribution of disordered solvent molecules removed by the
SQUEEZE process are included in the overall formula, formula weight, density,
F(000) etc. The output of the PLATON (generated as. sqf file) is
also appended to the bottom of the CIF.
;
_vrf_PLAT430_pdann
;
PROBLEM: Short Inter D...A Contact O27...O44 .. 2.74 Ang.
RESPONSE: The short contact is due to the hydrogen bonding between the lattice
included water and carboxylate. Since the hydrogen atom associated with the
lattice included water could not located in the differnece fourier map, it
shows as short contact alert.
;
# end Validation Reply Form
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 1.281 0.250 0.107 857.9 243.9
2 0.718 0.750 0.018 858.0 244.1
_platon_squeeze_details
; ?
;
_refine_diff_density_rms 0.048