#------------------------------------------------------------------------------
#$Date: 2013-08-28 13:42:33 +0300 (Wed, 28 Aug 2013) $
#$Revision: 88054 $
#$URL: file:///home/coder/svn-repositories/cod/hkl/2/23/78/2237882.hkl $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2237882_Fobs
loop_
_publ_author_name
'Kaur, Manpreet'
'Jasinski, Jerry P.'
'Luopa, Zane A.'
'Kumar, Neeraj'
'Patel, Nilesh G.'
'Gudaparthi, Omprakash'
'Yathirajan, H. S.'
_publ_contact_author_address
;
Department of Chemistry
Keene State College
229 Main Street
Keene, New Hampshire 03435, USA
;
_publ_contact_author_email jjasinski@keene.edu
_publ_contact_author_fax ?
_publ_contact_author_name 'Jasinski, Jerry P.'
_publ_contact_author_phone '603 358-2563'
_publ_section_title
;
Rupatadine
;
_journal_coden_ASTM ?
_journal_coeditor_code HG5317
_journal_coeditor_name ?
_journal_coeditor_notes ?
_journal_date_accepted ?
_journal_date_from_coeditor ?
_journal_date_printers_final ?
_journal_date_printers_first ?
_journal_date_proofs_in ?
_journal_date_proofs_out ?
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first o980
_journal_page_last ?
_journal_paper_category ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
_journal_techeditor_code ?
_journal_techeditor_notes ' ?'
_journal_volume 69
_journal_year 2013
_chemical_formula_moiety 'C26 H26 Cl N3'
_chemical_formula_sum 'C26 H26 Cl N3'
_chemical_formula_weight 415.95
_chemical_melting_point ?
_chemical_name_common Rupatadine
_chemical_name_systematic
;
8-Chloro-6,11-dihydro-11-[1-[(5-methyl-3-pyridinyl) methyl]-4-
piperidinylidene]-5H-benzo[5,6]cyclohepta[1,2-b]pyridine)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 21/n'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
_audit_creation_date 2013-05-5
_audit_creation_method
;
Olex2 1.2
(compiled Mar 21 2013 11:17:50, GUI svn.r4446)
;
_audit_update_record
;
2010-09-26 # Formatted by publCIF
2010-10-13 # Formatted by IUCr publCIF system
;
_cell_angle_alpha 90
_cell_angle_beta 90.874(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.2655(3)
_cell_length_b 11.3341(4)
_cell_length_c 18.8111(6)
_cell_measurement_reflns_used 4864
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 72.2007
_cell_measurement_theta_min 3.8969
_cell_volume 2188.43(11)
_computing_cell_refinement 'CrysAlisPro (Agilent, 2012)'
_computing_data_collection 'CrysAlisPro (Agilent, 2012)'
_computing_data_reduction 'CrysAlisRed (Agilent, 2012)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2008)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -1.00 36.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 30.0000 37
#__ type_ start__ end____ width___ exp.time_
2 omega -103.00 -21.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -57.0000 0.0000 82
#__ type_ start__ end____ width___ exp.time_
3 omega -108.00 -65.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -57.0000 90.0000 43
#__ type_ start__ end____ width___ exp.time_
4 omega -103.00 -32.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 178.0000 90.0000 71
#__ type_ start__ end____ width___ exp.time_
5 omega -112.00 -32.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -45.0000 -60.0000 80
#__ type_ start__ end____ width___ exp.time_
6 omega -59.00 -25.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -57.0000 90.0000 34
#__ type_ start__ end____ width___ exp.time_
7 omega -60.00 -30.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -61.0000 60.0000 30
#__ type_ start__ end____ width___ exp.time_
8 omega -110.00 -82.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -61.0000 60.0000 28
#__ type_ start__ end____ width___ exp.time_
9 omega 98.00 124.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 56.0000 37.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
10 omega -4.00 40.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 56.0000 -99.0000 -90.0000 44
#__ type_ start__ end____ width___ exp.time_
11 omega 32.00 58.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 56.0000 37.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
12 omega 38.00 116.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 56.0000 -131.0000 -29.0000 78
#__ type_ start__ end____ width___ exp.time_
13 omega 60.00 98.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -94.0000 0.0000 38
#__ type_ start__ end____ width___ exp.time_
14 omega 138.00 166.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 61.0000 -180.0000 28
#__ type_ start__ end____ width___ exp.time_
15 omega 58.00 108.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -94.0000 -150.0000 50
#__ type_ start__ end____ width___ exp.time_
16 omega 100.00 126.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 61.0000 -180.0000 26
#__ type_ start__ end____ width___ exp.time_
17 omega 42.00 85.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 30.0000 43
#__ type_ start__ end____ width___ exp.time_
18 omega 48.00 74.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 150.0000 26
#__ type_ start__ end____ width___ exp.time_
19 omega 60.00 103.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -94.0000 -60.0000 43
#__ type_ start__ end____ width___ exp.time_
20 omega 47.00 99.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 90.0000 52
#__ type_ start__ end____ width___ exp.time_
21 omega 39.00 65.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -30.0000 60.0000 26
#__ type_ start__ end____ width___ exp.time_
22 omega 41.00 111.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -111.0000 90.0000 70
#__ type_ start__ end____ width___ exp.time_
23 omega 84.00 111.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 30.0000 -60.0000 27
#__ type_ start__ end____ width___ exp.time_
24 omega 119.00 171.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 30.0000 -60.0000 52
#__ type_ start__ end____ width___ exp.time_
25 omega 129.00 178.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 77.0000 120.0000 49
#__ type_ start__ end____ width___ exp.time_
26 omega 41.00 95.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 -180.0000 54
#__ type_ start__ end____ width___ exp.time_
27 omega 41.00 96.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 -30.0000 55
#__ type_ start__ end____ width___ exp.time_
28 omega 39.00 173.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 0.0000 -90.0000 134
#__ type_ start__ end____ width___ exp.time_
29 omega 44.00 93.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -45.0000 -120.0000 49
#__ type_ start__ end____ width___ exp.time_
30 omega 54.00 108.00 1.0000 1.0000
omega____ theta____ kappa____ phi______ frames
- 112.0000 -94.0000 120.0000 54
;
_diffrn_measurement_device_type 'Xcalibur, Eos, Gemini'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0166252000
_diffrn_orient_matrix_UB_12 -0.0047910000
_diffrn_orient_matrix_UB_13 0.0815423000
_diffrn_orient_matrix_UB_21 0.1486551000
_diffrn_orient_matrix_UB_22 -0.0118375000
_diffrn_orient_matrix_UB_23 -0.0080349000
_diffrn_orient_matrix_UB_31 0.0136574000
_diffrn_orient_matrix_UB_32 0.1351137000
_diffrn_orient_matrix_UB_33 0.0022603000
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_R_equivalents 0.0264
_diffrn_reflns_av_unetI/netI 0.0240
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 13849
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 72.349
_diffrn_reflns_theta_min 4.555
_diffrn_source 'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 1.666
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.67287
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro and CrysAlisRed, Agilent (2012).
;
_exptl_crystal_colour 'clear orangish orange'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier orangish
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.262
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description irregular
_exptl_crystal_F_000 880
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.22
_refine_diff_density_max 0.222
_refine_diff_density_min -0.291
_refine_diff_density_rms 0.036
_refine_ls_extinction_coef 0.0043(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 273
_refine_ls_number_reflns 4281
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0498
_refine_ls_R_factor_gt 0.0412
_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^)+(0.0622P)^2^+0.3855P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1144
_refine_ls_wR_factor_ref 0.1222
_reflns_Friedel_coverage 0.000
_reflns_number_gt 3565
_reflns_number_total 4281
_reflns_threshold_expression 'I > 2\s(I)'
_[local]_cod_data_source_file hg5317Isup2.hkl
_[local]_cod_data_source_block I
#BEGIN Tags that were not found in dictionaries:
_publ_section_related_literature
;
For related pharmacological importance of rupatidine, see: Kean &
Plosker (2007); Merlos et al. (1997); Mullol et al.
(2008); Picado (2006).
For the reported synthesis methodology of rupatadine see:
Agarwal et al. (2008).
For bond lengths, see: Allen et al. (1987).
;
_chemical_oxdiff_formula 'C24 H25 N3 Cl'
_chemical_oxdiff_usercomment 'Yathi's HSY-579'
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_reflns_friedel_fraction_full .
_reflns_friedel_fraction_max .
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 66.97
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C4(H4A,H4B), C5(H5A,H5B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
C19(H19A,H19B), C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C22(H22), C23(H23),
C25(H25)
2.c Idealised Me refined as rotating group:
C26(H26A,H26B,H26C)
;
_shelx_estimated_absorpt_t_max ?
_shelx_estimated_absorpt_t_min ?
_shelx_res_file
;
TITL HSY-579 in P21/n #14
CELL 1.54184 10.26549 11.33411 18.81115 90 90.8743 90
ZERR 4 0.00029 0.00036 0.00055 0 0.0026 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N Cl
UNIT 104 104 12 4
L.S. 35
PLAN 10
TEMP -100(2)
HTAB C19 N1
REM reset to P21/n #14
BOND
fmap 2
ACTA
OMIT -1 0 1
REM E:/Chem-461%20Unknowns-2013/HSY-579-jpj/olex2_HSY-579-Loupa/HSY-579.h
REM kl
WGHT 0.062200 0.385500
EXTI 0.004253
FVAR 6.97902
CL1 4 0.214478 0.234989 0.095661 11.00000 0.05739 0.11784 =
0.07217 -0.00914 -0.00973 -0.03120
N1 3 0.765964 0.402493 0.353263 11.00000 0.04623 0.06039 =
0.03856 0.00162 0.00250 0.00546
N2 3 0.988908 0.589915 0.106390 11.00000 0.03415 0.04893 =
0.03443 -0.00080 0.00443 -0.00185
N3 3 1.296109 0.885577 0.145242 11.00000 0.07115 0.06249 =
0.07164 -0.01748 0.00501 -0.01656
C1 1 0.699929 0.440013 0.230530 11.00000 0.03912 0.04197 =
0.03485 0.00151 0.00341 -0.00045
C2 1 0.695964 0.469807 0.308012 11.00000 0.03833 0.04597 =
0.03554 0.00197 0.00559 -0.00521
C3 1 0.619656 0.564961 0.329548 11.00000 0.04566 0.04444 =
0.04297 -0.00077 0.00665 -0.00435
C4 1 0.544860 0.634271 0.274223 11.00000 0.06051 0.04020 =
0.05226 0.00353 0.00791 0.00260
AFIX 23
H4A 2 0.603842 0.654955 0.234981 11.00000 -1.20000
H4B 2 0.513708 0.708695 0.295643 11.00000 -1.20000
AFIX 0
C5 1 0.428401 0.565860 0.244095 11.00000 0.04763 0.05156 =
0.04689 0.01075 0.00510 0.00870
AFIX 23
H5A 2 0.369282 0.548767 0.283890 11.00000 -1.20000
H5B 2 0.380764 0.618658 0.210803 11.00000 -1.20000
AFIX 0
C6 1 0.453653 0.450935 0.205640 11.00000 0.04075 0.05050 =
0.03644 0.00986 0.00488 -0.00100
C7 1 0.574784 0.393373 0.199471 11.00000 0.03957 0.04591 =
0.03296 0.00632 0.00497 -0.00404
C8 1 0.760558 0.430094 0.422449 11.00000 0.06234 0.07356 =
0.03669 0.00426 -0.00116 0.00518
AFIX 43
H8 2 0.810074 0.383839 0.455169 11.00000 -1.20000
AFIX 0
C9 1 0.687580 0.521390 0.448840 11.00000 0.07298 0.07887 =
0.03617 -0.01068 0.00477 0.00158
AFIX 43
H9 2 0.686333 0.537311 0.498407 11.00000 -1.20000
AFIX 0
C10 1 0.616189 0.589301 0.401465 11.00000 0.06289 0.05553 =
0.04927 -0.01216 0.00835 0.00247
AFIX 43
H10 2 0.564669 0.652773 0.418289 11.00000 -1.20000
AFIX 0
C11 1 0.344139 0.399084 0.173495 11.00000 0.03920 0.07056 =
0.04584 0.00872 0.00329 -0.00305
AFIX 43
H11 2 0.261991 0.437153 0.176697 11.00000 -1.20000
AFIX 0
C12 1 0.353048 0.293976 0.137309 11.00000 0.04485 0.07172 =
0.04274 0.00556 -0.00173 -0.01733
C13 1 0.469340 0.233966 0.132723 11.00000 0.05982 0.05421 =
0.04347 -0.00124 0.00176 -0.01226
AFIX 43
H13 2 0.474427 0.160399 0.108724 11.00000 -1.20000
AFIX 0
C14 1 0.578837 0.284667 0.164367 11.00000 0.04491 0.04952 =
0.04255 0.00190 0.00369 -0.00142
AFIX 43
H14 2 0.659579 0.243987 0.162092 11.00000 -1.20000
AFIX 0
C15 1 0.808236 0.455285 0.192644 11.00000 0.03859 0.04574 =
0.03602 -0.00076 0.00343 -0.00224
C16 1 0.817021 0.437183 0.113340 11.00000 0.04511 0.05842 =
0.03703 -0.00777 0.00747 -0.01055
AFIX 23
H16A 2 0.730218 0.415406 0.093795 11.00000 -1.20000
H16B 2 0.877850 0.371602 0.103516 11.00000 -1.20000
AFIX 0
C17 1 0.864461 0.548776 0.077145 11.00000 0.03869 0.06078 =
0.03427 -0.00204 0.00297 -0.00504
AFIX 23
H17A 2 0.873842 0.533324 0.025678 11.00000 -1.20000
H17B 2 0.798423 0.611641 0.082646 11.00000 -1.20000
AFIX 0
C18 1 0.975941 0.613140 0.182773 11.00000 0.04177 0.05522 =
0.03642 -0.00511 0.00244 -0.00721
AFIX 23
H18A 2 0.910804 0.676356 0.189700 11.00000 -1.20000
H18B 2 1.060447 0.641238 0.202370 11.00000 -1.20000
AFIX 0
C19 1 0.934172 0.503515 0.222985 11.00000 0.03941 0.05637 =
0.03636 0.00115 0.00227 -0.00362
AFIX 23
H19A 2 1.003000 0.442628 0.219891 11.00000 -1.20000
H19B 2 0.922715 0.523306 0.273767 11.00000 -1.20000
AFIX 0
C20 1 1.026330 0.697421 0.068618 11.00000 0.04110 0.05402 =
0.04356 0.00625 0.00211 -0.00028
AFIX 23
H20A 2 0.963093 0.760619 0.079457 11.00000 -1.20000
H20B 2 1.021523 0.682330 0.016808 11.00000 -1.20000
AFIX 0
C21 1 1.161190 0.739616 0.087906 11.00000 0.04426 0.04474 =
0.03484 0.00523 0.00484 -0.00376
C22 1 1.179783 0.841456 0.127069 11.00000 0.05863 0.05501 =
0.05632 -0.00884 0.01101 -0.00352
AFIX 43
H22 2 1.104637 0.882922 0.142094 11.00000 -1.20000
AFIX 0
C23 1 1.399328 0.826019 0.122889 11.00000 0.05314 0.06895 =
0.05890 0.00071 -0.00240 -0.02268
AFIX 43
H23 2 1.483060 0.856319 0.134977 11.00000 -1.20000
AFIX 0
C24 1 1.393721 0.722664 0.083128 11.00000 0.04364 0.05985 =
0.04202 0.00964 0.00370 -0.00505
C25 1 1.270984 0.679320 0.066254 11.00000 0.04695 0.04719 =
0.03559 0.00072 0.00209 -0.00269
AFIX 43
H25 2 1.262112 0.608261 0.039837 11.00000 -1.20000
AFIX 0
C26 1 1.515317 0.659059 0.061509 11.00000 0.04562 0.08817 =
0.07581 0.01212 0.00777 0.00454
AFIX 137
H26A 2 1.505618 0.574489 0.070895 11.00000 -1.50000
H26B 2 1.589927 0.689752 0.088864 11.00000 -1.50000
H26C 2 1.529694 0.671461 0.010671 11.00000 -1.50000
AFIX 0
HKLF 4
REM HSY-579 in P21/n #14
REM R1 = 0.0412 for 3565 Fo > 4sig(Fo) and 0.0498 for all 4281 data
REM 273 parameters refined using 0 restraints
END
WGHT 0.0616 0.3876
REM Highest difference peak 0.222, deepest hole -0.291, 1-sigma level 0.036
Q1 1 0.5197 0.4358 0.1992 11.00000 0.05 0.22
Q2 1 1.4960 0.5977 0.0236 11.00000 0.05 0.21
Q3 1 0.1886 0.2812 0.1320 11.00000 0.05 0.18
Q4 1 1.0978 0.7227 0.0740 11.00000 0.05 0.18
Q5 1 0.6332 0.4265 0.2120 11.00000 0.05 0.18
Q6 1 0.7000 0.4568 0.2699 11.00000 0.05 0.18
Q7 1 0.8660 0.4897 0.2103 11.00000 0.05 0.17
Q8 1 0.2798 0.1882 0.1068 11.00000 0.05 0.16
Q9 1 0.7707 0.4037 0.2205 11.00000 0.05 0.16
Q10 1 0.7374 0.4818 0.2079 11.00000 0.05 0.16
REM The information below was added by Olex2.
REM
REM R1 = 0.0412 for 3565 Fo > 4sig(Fo) and 0.0498 for all 14247 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.22, deepest hole -0.29
REM Mean Shift 0, Max Shift 0.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0498
REM R1_gt = 0.0412
REM wR_ref = 0.1222
REM GOOF = 1.053
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 14247
REM Reflections_gt = 3565
REM Parameters = n/a
REM Hole = 0.22
REM Peak = -0.29
REM Flack = n/a
;
_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.
;
_shelxl_version_number 2012-9
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Cl1 Cl 0.21448(5) 0.23499(6) 0.09566(3) 0.0826(2) Uani 1 1 d . . . . .
N1 N 0.76596(13) 0.40249(13) 0.35326(7) 0.0484(3) Uani 1 1 d . . . . .
N2 N 0.98891(11) 0.58992(11) 0.10639(6) 0.0391(3) Uani 1 1 d . . . . .
N3 N 1.29611(17) 0.88558(15) 0.14524(10) 0.0684(5) Uani 1 1 d . . . . .
C1 C 0.69993(14) 0.44001(13) 0.23053(7) 0.0386(3) Uani 1 1 d . . . . .
C2 C 0.69596(14) 0.46981(14) 0.30801(8) 0.0399(3) Uani 1 1 d . . . . .
C3 C 0.61966(15) 0.56496(14) 0.32955(8) 0.0443(4) Uani 1 1 d . . . . .
C4 C 0.54486(17) 0.63427(15) 0.27422(9) 0.0509(4) Uani 1 1 d . . . . .
H4A H 0.6038 0.6550 0.2350 0.061 Uiso 1 1 calc R U . . .
H4B H 0.5137 0.7087 0.2956 0.061 Uiso 1 1 calc R U . . .
C5 C 0.42840(16) 0.56586(15) 0.24409(9) 0.0486(4) Uani 1 1 d . . . . .
H5A H 0.3693 0.5488 0.2839 0.058 Uiso 1 1 calc R U . . .
H5B H 0.3808 0.6187 0.2108 0.058 Uiso 1 1 calc R U . . .
C6 C 0.45365(15) 0.45093(14) 0.20564(8) 0.0425(3) Uani 1 1 d . . . . .
C7 C 0.57478(14) 0.39337(14) 0.19947(7) 0.0394(3) Uani 1 1 d . . . . .
C8 C 0.76056(19) 0.43009(18) 0.42245(9) 0.0575(5) Uani 1 1 d . . . . .
H8 H 0.8101 0.3838 0.4552 0.069 Uiso 1 1 calc R U . . .
C9 C 0.6876(2) 0.52139(19) 0.44884(9) 0.0626(5) Uani 1 1 d . . . . .
H9 H 0.6863 0.5373 0.4984 0.075 Uiso 1 1 calc R U . . .
C10 C 0.61619(18) 0.58930(16) 0.40147(9) 0.0558(4) Uani 1 1 d . . . . .
H10 H 0.5647 0.6528 0.4183 0.067 Uiso 1 1 calc R U . . .
C11 C 0.34414(16) 0.39908(17) 0.17349(9) 0.0518(4) Uani 1 1 d . . . . .
H11 H 0.2620 0.4372 0.1767 0.062 Uiso 1 1 calc R U . . .
C12 C 0.35305(16) 0.29398(17) 0.13731(9) 0.0531(4) Uani 1 1 d . . . . .
C13 C 0.46934(18) 0.23397(16) 0.13272(9) 0.0525(4) Uani 1 1 d . . . . .
H13 H 0.4744 0.1604 0.1087 0.063 Uiso 1 1 calc R U . . .
C14 C 0.57884(16) 0.28467(15) 0.16437(8) 0.0456(4) Uani 1 1 d . . . . .
H14 H 0.6596 0.2440 0.1621 0.055 Uiso 1 1 calc R U . . .
C15 C 0.80824(14) 0.45529(14) 0.19264(8) 0.0401(3) Uani 1 1 d . . . . .
C16 C 0.81702(16) 0.43718(15) 0.11334(8) 0.0468(4) Uani 1 1 d . . . . .
H16A H 0.7302 0.4154 0.0938 0.056 Uiso 1 1 calc R U . . .
H16B H 0.8779 0.3716 0.1035 0.056 Uiso 1 1 calc R U . . .
C17 C 0.86446(14) 0.54878(15) 0.07714(8) 0.0446(4) Uani 1 1 d . . . . .
H17A H 0.8738 0.5333 0.0257 0.053 Uiso 1 1 calc R U . . .
H17B H 0.7984 0.6116 0.0826 0.053 Uiso 1 1 calc R U . . .
C18 C 0.97594(15) 0.61314(15) 0.18277(8) 0.0445(4) Uani 1 1 d . . . . .
H18A H 0.9108 0.6764 0.1897 0.053 Uiso 1 1 calc R U . . .
H18B H 1.0604 0.6412 0.2024 0.053 Uiso 1 1 calc R U . . .
C19 C 0.93417(14) 0.50352(15) 0.22299(8) 0.0440(4) Uani 1 1 d . . . . .
H19A H 1.0030 0.4426 0.2199 0.053 Uiso 1 1 calc R U . . .
H19B H 0.9227 0.5233 0.2738 0.053 Uiso 1 1 calc R U . . .
C20 C 1.02633(15) 0.69742(15) 0.06862(8) 0.0462(4) Uani 1 1 d . . . . .
H20A H 0.9631 0.7606 0.0795 0.055 Uiso 1 1 calc R U . . .
H20B H 1.0215 0.6823 0.0168 0.055 Uiso 1 1 calc R U . . .
C21 C 1.16119(15) 0.73962(13) 0.08791(8) 0.0412(3) Uani 1 1 d . . . . .
C22 C 1.17978(18) 0.84146(16) 0.12707(10) 0.0566(4) Uani 1 1 d . . . . .
H22 H 1.1046 0.8829 0.1421 0.068 Uiso 1 1 calc R U . . .
C23 C 1.39933(18) 0.82602(18) 0.12289(10) 0.0604(5) Uani 1 1 d . . . . .
H23 H 1.4831 0.8563 0.1350 0.072 Uiso 1 1 calc R U . . .
C24 C 1.39372(16) 0.72266(16) 0.08313(9) 0.0485(4) Uani 1 1 d . . . . .
C25 C 1.27098(15) 0.67932(15) 0.06625(8) 0.0432(3) Uani 1 1 d . . . . .
H25 H 1.2621 0.6083 0.0398 0.052 Uiso 1 1 calc R U . . .
C26 C 1.51532(18) 0.6591(2) 0.06151(12) 0.0698(6) Uani 1 1 d . . . . .
H26A H 1.5056 0.5745 0.0709 0.105 Uiso 1 1 calc R U . . .
H26B H 1.5899 0.6898 0.0889 0.105 Uiso 1 1 calc R U . . .
H26C H 1.5297 0.6715 0.0107 0.105 Uiso 1 1 calc R U . . .
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
Cl1 0.0574(3) 0.1178(5) 0.0722(3) -0.0091(3) -0.0097(2) -0.0312(3)
N1 0.0462(7) 0.0604(8) 0.0386(7) 0.0016(6) 0.0025(5) 0.0055(6)
N2 0.0342(6) 0.0489(7) 0.0344(6) -0.0008(5) 0.0044(5) -0.0019(5)
N3 0.0712(11) 0.0625(10) 0.0716(11) -0.0175(8) 0.0050(8) -0.0166(8)
C1 0.0391(7) 0.0420(8) 0.0348(7) 0.0015(6) 0.0034(6) -0.0004(6)
C2 0.0383(7) 0.0460(8) 0.0355(7) 0.0020(6) 0.0056(6) -0.0052(6)
C3 0.0457(8) 0.0444(8) 0.0430(8) -0.0008(7) 0.0066(6) -0.0044(7)
C4 0.0605(10) 0.0402(8) 0.0523(9) 0.0035(7) 0.0079(7) 0.0026(7)
C5 0.0476(9) 0.0516(9) 0.0469(9) 0.0107(7) 0.0051(7) 0.0087(7)
C6 0.0408(8) 0.0505(9) 0.0364(7) 0.0099(6) 0.0049(6) -0.0010(6)
C7 0.0396(7) 0.0459(8) 0.0330(7) 0.0063(6) 0.0050(6) -0.0040(6)
C8 0.0623(11) 0.0736(12) 0.0367(8) 0.0043(8) -0.0012(7) 0.0052(9)
C9 0.0730(12) 0.0789(13) 0.0362(8) -0.0107(8) 0.0048(8) 0.0016(10)
C10 0.0629(11) 0.0555(10) 0.0493(9) -0.0122(8) 0.0083(8) 0.0025(8)
C11 0.0392(8) 0.0706(11) 0.0458(9) 0.0087(8) 0.0033(7) -0.0031(7)
C12 0.0449(9) 0.0717(12) 0.0427(8) 0.0056(8) -0.0017(7) -0.0173(8)
C13 0.0598(10) 0.0542(10) 0.0435(9) -0.0012(7) 0.0018(7) -0.0123(8)
C14 0.0449(8) 0.0495(9) 0.0426(8) 0.0019(7) 0.0037(6) -0.0014(7)
C15 0.0386(7) 0.0457(8) 0.0360(7) -0.0008(6) 0.0034(6) -0.0022(6)
C16 0.0451(8) 0.0584(10) 0.0370(8) -0.0078(7) 0.0075(6) -0.0105(7)
C17 0.0387(8) 0.0608(10) 0.0343(7) -0.0020(7) 0.0030(6) -0.0050(7)
C18 0.0418(8) 0.0552(9) 0.0364(7) -0.0051(7) 0.0024(6) -0.0072(7)
C19 0.0394(8) 0.0564(9) 0.0364(7) 0.0012(7) 0.0023(6) -0.0036(7)
C20 0.0411(8) 0.0540(9) 0.0436(8) 0.0062(7) 0.0021(6) -0.0003(7)
C21 0.0443(8) 0.0447(8) 0.0348(7) 0.0052(6) 0.0048(6) -0.0038(6)
C22 0.0586(10) 0.0550(10) 0.0563(10) -0.0088(8) 0.0110(8) -0.0035(8)
C23 0.0531(10) 0.0690(12) 0.0589(10) 0.0007(9) -0.0024(8) -0.0227(9)
C24 0.0436(8) 0.0598(10) 0.0420(8) 0.0096(7) 0.0037(6) -0.0051(7)
C25 0.0469(8) 0.0472(8) 0.0356(7) 0.0007(6) 0.0021(6) -0.0027(7)
C26 0.0456(10) 0.0882(15) 0.0758(13) 0.0121(11) 0.0078(9) 0.0045(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C8 N1 C2 116.94(15) . . ?
C17 N2 C18 109.52(11) . . ?
C17 N2 C20 108.51(12) . . ?
C20 N2 C18 110.72(12) . . ?
C23 N3 C22 116.29(16) . . ?
C2 C1 C7 115.02(12) . . ?
C15 C1 C2 121.55(13) . . ?
C15 C1 C7 123.42(13) . . ?
N1 C2 C1 117.81(13) . . ?
N1 C2 C3 123.49(14) . . ?
C3 C2 C1 118.70(14) . . ?
C2 C3 C4 119.01(14) . . ?
C10 C3 C2 117.46(15) . . ?
C10 C3 C4 123.53(15) . . ?
C3 C4 C5 112.33(13) . . ?
C6 C5 C4 118.39(13) . . ?
C7 C6 C5 126.49(14) . . ?
C11 C6 C5 115.21(14) . . ?
C11 C6 C7 118.30(15) . . ?
C6 C7 C1 123.78(14) . . ?
C14 C7 C1 117.58(13) . . ?
C14 C7 C6 118.61(14) . . ?
N1 C8 C9 123.86(17) . . ?
C8 C9 C10 118.27(16) . . ?
C9 C10 C3 119.98(17) . . ?
C12 C11 C6 121.26(16) . . ?
C11 C12 Cl1 119.58(14) . . ?
C11 C12 C13 121.51(15) . . ?
C13 C12 Cl1 118.91(15) . . ?
C12 C13 C14 117.74(17) . . ?
C13 C14 C7 122.50(16) . . ?
C1 C15 C16 124.75(14) . . ?
C1 C15 C19 123.97(13) . . ?
C19 C15 C16 111.07(12) . . ?
C15 C16 C17 110.72(13) . . ?
N2 C17 C16 112.43(13) . . ?
N2 C18 C19 111.77(13) . . ?
C15 C19 C18 110.78(13) . . ?
N2 C20 C21 113.25(12) . . ?
C22 C21 C20 120.91(15) . . ?
C22 C21 C25 117.58(15) . . ?
C25 C21 C20 121.50(14) . . ?
N3 C22 C21 124.46(17) . . ?
N3 C23 C24 124.82(16) . . ?
C23 C24 C26 121.46(17) . . ?
C25 C24 C23 116.89(16) . . ?
C25 C24 C26 121.63(17) . . ?
C21 C25 C24 119.96(15) . . ?
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
Cl1 C12 1.7465(17) . ?
N1 C2 1.343(2) . ?
N1 C8 1.341(2) . ?
N2 C17 1.4597(18) . ?
N2 C18 1.4688(18) . ?
N2 C20 1.465(2) . ?
N3 C22 1.334(2) . ?
N3 C23 1.330(3) . ?
C1 C2 1.4973(19) . ?
C1 C7 1.499(2) . ?
C1 C15 1.341(2) . ?
C2 C3 1.397(2) . ?
C3 C4 1.505(2) . ?
C3 C10 1.382(2) . ?
C4 C5 1.527(2) . ?
C5 C6 1.514(2) . ?
C6 C7 1.411(2) . ?
C6 C11 1.398(2) . ?
C7 C14 1.399(2) . ?
C8 C9 1.375(3) . ?
C9 C10 1.380(3) . ?
C11 C12 1.376(3) . ?
C12 C13 1.378(3) . ?
C13 C14 1.388(2) . ?
C15 C16 1.510(2) . ?
C15 C19 1.508(2) . ?
C16 C17 1.520(2) . ?
C18 C19 1.520(2) . ?
C20 C21 1.504(2) . ?
C21 C22 1.381(2) . ?
C21 C25 1.385(2) . ?
C23 C24 1.391(3) . ?
C24 C25 1.385(2) . ?
C24 C26 1.503(2) . ?
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
C19 H19B N1 0.99 2.60 3.229(2) 121.3 .
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 -2 217450 1191.34 2
0 0 -3 1046.3 110.098 2
0 0 -4 931554 3528.55 2
0 0 -5 253.311 85.6389 2
0 0 -6 452296 2981.51 2
0 0 6 453863 2899.93 11
0 0 -7 -10.7964 72.6139 2
0 0 7 317.439 95.6396 11
0 0 -8 85818.4 1523.63 2
0 0 8 81787.7 1483.74 11
0 0 -9 -66.4729 100.017 5
0 0 -9 21.0451 94.1748 2
0 0 -10 86590.9 1743.6 2
0 0 -10 85755.5 1557.15 5
0 0 -11 -81.456 133.671 2
0 0 -11 -91.9973 89.4501 5
0 0 -12 17790.7 773.899 5
0 0 -12 18550.8 895.978 2
0 0 -13 237.258 153.993 2
0 0 -13 -3.07951 69.378 5
0 0 -14 6520.03 571.544 2
0 0 -15 133.13 139.371 4
0 0 -15 44.6487 107.841 2
0 0 -16 -7.78769 111.092 24
0 0 -17 -49.7401 108.228 24
0 0 18 3871.72 429.188 25
0 0 18 3183.45 433.393 28
0 0 18 3707.38 431.932 16
0 0 19 -94.037 146.69 28
0 0 19 -27.3611 94.8589 16
0 0 20 327.505 168.264 28
0 0 20 172.057 113.349 16
0 0 21 -41.5471 111.798 28
0 0 22 2054.83 269.301 28
0 0 23 -37.9335 63.8019 28
0 -1 0 49.1746 21.6196 1
0 1 -1 19185.3 295.848 4
0 -1 -1 20495.8 292.353 1
0 1 -2 12434.3 264.069 2
0 -1 -2 11939.6 283.277 2
0 1 -2 12333.2 299.552 4
0 -1 -3 26375.4 515.53 2
0 -1 -3 25835.9 394.103 8
0 1 -3 25618.7 517.518 4
0 1 -3 26761.1 484.864 2
0 -1 -4 422056 2406.69 2
0 -1 -4 404146 1884.86 8
0 -1 -5 118297 1449.26 2
0 -1 -5 113338 1159.14 8
0 1 -5 116042 1340.36 2
0 1 -6 16466.8 561.587 2
0 -1 -6 16887.7 613.677 2
0 -1 6 15807.6 575.067 11
0 1 -6 16428.9 460.95 5
0 -1 -7 321819 2857.65 2
0 -1 7 298041 2728.78 11
0 1 -7 304723 2636.34 2
0 1 -7 312782 2218.91 5
0 1 -8 8741.66 407.764 5
0 1 -8 8933.47 487.744 2
0 -1 8 8689.71 501.992 11
0 -1 -8 8866.82 512.998 2
0 -1 -9 51972.5 1293.18 2
0 1 -9 52145.8 1257.91 2
0 1 -9 52885.5 1064 5
0 -1 9 51502.5 1300.45 11
0 1 -10 33134 893.068 5
0 -1 -10 32640.7 1016.78 5
0 -1 -10 32222.8 1080.47 2
0 1 -10 33089.7 1062.95 2
0 -1 -11 14517.4 715.571 5
0 -1 -11 14677.7 772.901 2
0 1 -11 14282.9 738.883 2
0 -1 -12 39285.4 1219.12 5
0 1 -12 39589.2 1357.05 4
0 1 -12 40666 1304.48 2
0 -1 -12 39354.7 1322.83 2
0 1 -13 3304.36 392.537 2
0 1 -13 3283.62 405.824 4
0 -1 -13 2592.16 321.962 5
0 -1 -13 2692.82 370.875 2
0 1 -14 9239.88 704.897 4
0 -1 -14 8596.91 659.87 2
0 -1 -14 8255.16 597.51 5
0 1 -14 8939.31 665.855 2
0 -1 -15 -118.216 113.663 2
0 1 -15 369.815 140.01 4
0 1 -16 14932.2 867.453 24
0 -1 -16 16627.3 868.545 24
0 1 17 3262.14 408.904 25
0 -1 -17 2620.1 337.439 24
0 -1 17 3810.29 477.571 28
0 -1 18 14045.2 890.132 28
0 1 18 14658.4 849.692 25
0 1 18 13061.4 859.58 28
0 1 19 464.063 168.365 25
0 -1 19 257.448 148.631 16
0 1 19 276.557 182.324 28
0 -1 19 230.377 140.846 28
0 1 20 161.806 114.354 25
0 1 20 106.228 113.193 28
0 -1 20 12.8431 107.353 28
0 -1 20 130.165 104.663 16
0 1 21 1856.69 281.744 28
0 -1 21 2036.13 265.441 16
0 1 21 2399.65 272.187 25
0 -1 21 2072.27 299.059 28
0 -1 22 198.873 111.541 28
0 1 22 254.403 120.446 28
0 -1 22 153.744 70.6185 16
0 1 23 2694.24 237.75 28
0 -1 23 2581.65 235.427 28
0 -2 0 5866.97 199.925 1
0 2 0 5742.34 210.32 4
0 -2 -1 44168.9 549.989 1
0 2 -1 41077.4 566.886 4
0 -2 -2 465976 1959.7 2
0 2 -2 458259 2108.14 4
0 2 -3 68634.9 908.694 4
0 -2 -3 69951.1 880.552 2
0 -2 -4 575319 2037.88 8
0 -2 4 549626 2964.46 11
0 -2 -4 564185 2885.77 2
0 -2 -5 627718 3418.4 2
0 -2 -5 624756 2498 8
0 2 -5 601098 3017.55 2
0 -2 5 622551 3513.31 11
0 -2 -6 60655.6 869.317 8
0 2 -6 60391 1159.11 4
0 -2 6 62894.9 1217.15 11
0 2 -6 62075.4 754.906 5
0 -2 -6 63039.9 1186.62 2
0 2 -6 62236.2 1073.56 2
0 -2 7 32240.4 932.65 11
0 2 -7 30878.7 608.325 5
0 2 -7 30728.9 898.697 4
0 -2 -7 32341 942.48 2
0 2 -7 30092.2 818.251 2
0 -2 -8 34522.9 1036.28 2
0 2 -8 32368.4 916.726 2
0 2 -8 32108.3 986.042 4
0 -2 8 32405.2 1001.09 11
0 2 -9 89114.8 1627 2
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