#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:52:33 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257544 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705283.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7705283
loop_
_publ_author_name
'Guo, Yuan-Yuan'
'Lightfoot, Philip'
_publ_section_title
;
Structural diversity of lead halide chain compounds, APbX3,
templated by isomeric molecular cations.
;
_journal_issue 36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 12767
_journal_page_last 12775
_journal_paper_doi 10.1039/d0dt02782k
_journal_volume 49
_journal_year 2020
_chemical_formula_moiety 'Br3 Pb, C9 H8 N'
_chemical_formula_sum 'C9 H8 Br3 N Pb'
_chemical_formula_weight 577.08
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2020-08-07 deposited with the CCDC. 2020-08-27 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 99.068(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.3634(4)
_cell_length_b 22.5833(18)
_cell_length_c 13.1074(11)
_cell_measurement_reflns_used 952
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.4
_cell_volume 1275.46(19)
_computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material 'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature 298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0609
_diffrn_reflns_av_unetI/netI 0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 12963
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.484
_diffrn_reflns_theta_min 2.394
_diffrn_source 'Sealed Tube'
_exptl_absorpt_coefficient_mu 22.589
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.571
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 3.005
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 1024
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_refine_diff_density_max 1.295
_refine_diff_density_min -1.446
_refine_diff_density_rms 0.152
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.870
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 127
_refine_ls_number_reflns 2918
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.870
_refine_ls_R_factor_all 0.0407
_refine_ls_R_factor_gt 0.0250
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0484
_refine_ls_wR_factor_ref 0.0507
_reflns_Friedel_coverage 0.000
_reflns_number_gt 2189
_reflns_number_total 2918
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0dt02782k2.cif
_cod_data_source_block shelx_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:
data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.
Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas
Adding full bibliography for 7705282--7705287.cif.
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 7705283
_shelx_shelxl_version_number 2018/3
_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.
;
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/n
shelx.res
created by SHELXL-2018/3 at 14:36:36 on 10-Jun-2020
REM Old TITL RC14RTB
REM SHELXT solution in P2(1)/n: R1 0.068, Rweak 0.004, Alpha 0.046
REM 0.188 for 82 systematic absences, Orientation as input
REM Formula found by SHELXT: Pb Br3 N C9
CELL 0.71075 4.3634 22.5833 13.1074 90.000 99.068 90.000
ZERR 4.000 0.0004 0.0018 0.0011 0.000 0.008 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC PB BR N C H
UNIT 4 12 4 36 32
L.S. 10
BOND
HTAB
HTAB N1 Br1
ACTA
LIST 4
FMAP 2
PLAN 10
WGHT 0.021000
FVAR 0.19110
PB1 1 0.701912 0.532249 0.857410 11.00000 0.03085 0.03319 =
0.03028 0.00180 0.00409 -0.00108
BR1 2 0.609706 0.509917 0.642708 11.00000 0.05737 0.04089 =
0.03323 -0.00433 0.00095 0.01034
BR2 2 1.191380 0.622858 0.827779 11.00000 0.03772 0.03201 =
0.05530 -0.00060 0.00764 -0.00184
BR3 2 0.225709 0.439808 0.893657 11.00000 0.04649 0.03248 =
0.04571 0.00336 0.00636 -0.00361
N1 3 0.198214 0.618533 0.516914 11.00000 0.05565 0.03499 =
0.07531 0.01026 0.01213 0.00879
AFIX 43
H1 5 0.266802 0.589514 0.556523 11.00000 -1.20000
AFIX 0
C1 4 -0.020625 0.607963 0.437763 11.00000 0.05230 0.05480 =
0.09966 -0.02886 0.01498 -0.00076
AFIX 43
H2 5 -0.093507 0.569547 0.425033 11.00000 -1.20000
AFIX 0
C2 4 -0.143485 0.653627 0.373171 11.00000 0.07118 0.09578 =
0.05608 -0.00969 0.00663 0.02276
AFIX 43
H3 5 -0.300208 0.646181 0.317881 11.00000 -1.20000
AFIX 0
C3 4 -0.031785 0.709281 0.391804 11.00000 0.06353 0.06276 =
0.05304 0.01307 0.01249 0.02029
AFIX 43
H4 5 -0.110452 0.740028 0.348190 11.00000 -1.20000
AFIX 0
C4 4 0.199600 0.720969 0.475566 11.00000 0.04732 0.04339 =
0.04668 0.01373 0.01846 0.01323
C5 4 0.323912 0.778039 0.499849 11.00000 0.06251 0.03384 =
0.09327 0.02128 0.02716 0.01518
AFIX 43
H5 5 0.245493 0.810587 0.460737 11.00000 -1.20000
AFIX 0
C6 4 0.556548 0.785123 0.579903 11.00000 0.06240 0.03847 =
0.11702 -0.00363 0.03178 -0.00111
AFIX 43
H6 5 0.640945 0.822558 0.594554 11.00000 -1.20000
AFIX 0
C7 4 0.672079 0.737097 0.640936 11.00000 0.05393 0.05803 =
0.06543 -0.00240 0.01092 0.00326
AFIX 43
H7 5 0.830820 0.743223 0.696165 11.00000 -1.20000
AFIX 0
C8 4 0.558446 0.681720 0.621643 11.00000 0.05492 0.04868 =
0.04824 0.01403 0.01425 0.00939
AFIX 43
H8 5 0.637342 0.649963 0.662765 11.00000 -1.20000
AFIX 0
C9 4 0.321248 0.673567 0.538940 11.00000 0.04705 0.03208 =
0.04992 0.00893 0.02299 0.01088
HKLF 4
REM shelxt_a.res in P2(1)/n
REM wR2 = 0.0507, GooF = S = 0.870, Restrained GooF = 0.870 for all data
REM R1 = 0.0250 for 2189 Fo > 4sig(Fo) and 0.0407 for all 2918 data
REM 127 parameters refined using 0 restraints
END
WGHT 0.0210 0.0000
REM Instructions for potential hydrogen bonds
HTAB N1 Br1
EQIV $3 -x+1, -y+1, -z+1
HTAB C1 Br1_$3
REM Highest difference peak 1.295, deepest hole -1.446, 1-sigma level 0.152
Q1 1 0.6989 0.5763 0.8585 11.00000 0.05 1.30
Q2 1 0.7109 0.4894 0.8577 11.00000 0.05 1.25
Q3 1 0.6631 0.5314 0.7919 11.00000 0.05 1.00
Q4 1 0.7366 0.5326 0.9233 11.00000 0.05 0.99
Q5 1 0.9313 0.5717 0.8349 11.00000 0.05 0.84
Q6 1 0.4979 0.4906 0.8822 11.00000 0.05 0.81
Q7 1 0.8801 0.4936 0.8185 11.00000 0.05 0.74
Q8 1 0.2267 0.4374 0.8289 11.00000 0.05 0.68
Q9 1 0.5436 0.5676 0.8927 11.00000 0.05 0.64
Q10 1 1.1820 0.6234 0.8927 11.00000 0.05 0.59
;
_shelx_res_checksum 84823
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
Pb1 Pb 0.70191(4) 0.53225(2) 0.85741(2) 0.03152(7) Uani 1 1 d . . . . .
Br1 Br 0.60971(14) 0.50992(3) 0.64271(4) 0.04450(15) Uani 1 1 d . . . . .
Br2 Br 1.19138(12) 0.62286(3) 0.82778(5) 0.04164(14) Uani 1 1 d . . . . .
Br3 Br 0.22571(13) 0.43981(3) 0.89366(4) 0.04166(14) Uani 1 1 d . . . . .
N1 N 0.1982(12) 0.6185(2) 0.5169(4) 0.0551(14) Uani 1 1 d . . . . .
H1 H 0.266802 0.589514 0.556523 0.066 Uiso 1 1 calc R U . . .
C1 C -0.0206(15) 0.6080(3) 0.4378(6) 0.069(2) Uani 1 1 d . . . . .
H2 H -0.093507 0.569547 0.425033 0.082 Uiso 1 1 calc R U . . .
C2 C -0.1435(18) 0.6536(4) 0.3732(6) 0.075(2) Uani 1 1 d . . . . .
H3 H -0.300208 0.646181 0.317881 0.090 Uiso 1 1 calc R U . . .
C3 C -0.0318(15) 0.7093(4) 0.3918(5) 0.0594(18) Uani 1 1 d . . . . .
H4 H -0.110452 0.740028 0.348190 0.071 Uiso 1 1 calc R U . . .
C4 C 0.1996(13) 0.7210(3) 0.4756(5) 0.0446(15) Uani 1 1 d . . . . .
C5 C 0.3239(16) 0.7780(3) 0.4998(6) 0.0616(19) Uani 1 1 d . . . . .
H5 H 0.245493 0.810587 0.460737 0.074 Uiso 1 1 calc R U . . .
C6 C 0.5565(17) 0.7851(3) 0.5799(7) 0.071(2) Uani 1 1 d . . . . .
H6 H 0.640945 0.822558 0.594554 0.085 Uiso 1 1 calc R U . . .
C7 C 0.6721(16) 0.7371(3) 0.6409(5) 0.0590(18) Uani 1 1 d . . . . .
H7 H 0.830820 0.743223 0.696165 0.071 Uiso 1 1 calc R U . . .
C8 C 0.5584(14) 0.6817(3) 0.6216(5) 0.0500(16) Uani 1 1 d . . . . .
H8 H 0.637342 0.649963 0.662765 0.060 Uiso 1 1 calc R U . . .
C9 C 0.3212(13) 0.6736(3) 0.5389(5) 0.0414(14) 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
Pb1 0.03085(10) 0.03319(12) 0.03028(11) 0.00180(9) 0.00409(7) -0.00108(9)
Br1 0.0574(3) 0.0409(3) 0.0332(3) -0.0043(2) 0.0009(3) 0.0103(3)
Br2 0.0377(3) 0.0320(3) 0.0553(4) -0.0006(3) 0.0076(3) -0.0018(2)
Br3 0.0465(3) 0.0325(3) 0.0457(3) 0.0034(3) 0.0064(2) -0.0036(3)
N1 0.056(3) 0.035(3) 0.075(4) 0.010(3) 0.012(3) 0.009(3)
C1 0.052(4) 0.055(5) 0.100(6) -0.029(4) 0.015(4) -0.001(4)
C2 0.071(5) 0.096(7) 0.056(5) -0.010(5) 0.007(4) 0.023(5)
C3 0.064(4) 0.063(5) 0.053(4) 0.013(4) 0.012(3) 0.020(4)
C4 0.047(3) 0.043(4) 0.047(4) 0.014(3) 0.018(3) 0.013(3)
C5 0.063(4) 0.034(4) 0.093(6) 0.021(4) 0.027(4) 0.015(3)
C6 0.062(5) 0.038(4) 0.117(7) -0.004(4) 0.032(5) -0.001(4)
C7 0.054(4) 0.058(5) 0.065(5) -0.002(4) 0.011(3) 0.003(4)
C8 0.055(4) 0.049(4) 0.048(4) 0.014(3) 0.014(3) 0.009(3)
C9 0.047(3) 0.032(3) 0.050(4) 0.009(3) 0.023(3) 0.011(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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'
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
Br1 Pb1 Br2 90.374(18) . 1_455 ?
Br1 Pb1 Br2 89.166(19) . . ?
Br2 Pb1 Br2 92.681(18) 1_455 . ?
Br1 Pb1 Br3 92.27(2) . . ?
Br2 Pb1 Br3 88.667(18) 1_455 . ?
Br2 Pb1 Br3 178.024(17) . . ?
Br1 Pb1 Br3 91.053(18) . 1_655 ?
Br2 Pb1 Br3 178.562(17) 1_455 1_655 ?
Br2 Pb1 Br3 87.509(17) . 1_655 ?
Br3 Pb1 Br3 91.107(18) . 1_655 ?
Pb1 Br2 Pb1 92.681(18) 1_655 . ?
Pb1 Br3 Pb1 91.108(18) . 1_455 ?
C1 N1 C9 122.9(6) . . ?
N1 C1 C2 120.6(7) . . ?
C3 C2 C1 119.1(7) . . ?
C2 C3 C4 120.8(7) . . ?
C3 C4 C9 118.7(6) . . ?
C3 C4 C5 123.6(6) . . ?
C9 C4 C5 117.7(6) . . ?
C6 C5 C4 119.8(6) . . ?
C5 C6 C7 120.9(7) . . ?
C8 C7 C6 121.5(7) . . ?
C7 C8 C9 118.3(6) . . ?
N1 C9 C8 120.4(6) . . ?
N1 C9 C4 117.9(6) . . ?
C8 C9 C4 121.7(6) . . ?
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
Pb1 Br1 2.8247(6) . ?
Pb1 Br2 3.0046(6) 1_455 ?
Pb1 Br2 3.0267(6) . ?
Pb1 Br3 3.0352(6) . ?
Pb1 Br3 3.0766(6) 1_655 ?
N1 C1 1.316(9) . ?
N1 C9 1.367(8) . ?
C1 C2 1.387(10) . ?
C2 C3 1.356(10) . ?
C3 C4 1.395(9) . ?
C4 C9 1.407(8) . ?
C4 C5 1.415(9) . ?
C5 C6 1.350(10) . ?
C6 C7 1.394(10) . ?
C7 C8 1.354(9) . ?
C8 C9 1.388(8) . ?
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
_geom_hbond_publ_flag
N1 H1 Br1 0.86 2.49 3.321(5) 161.8 . yes