#------------------------------------------------------------------------------
#$Date: 2019-07-30 02:15:55 +0200 (Tue 30 de Jul de 2019) $
#$Revision: 217290 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/39/7123922.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_7123922
loop_
_publ_author_name
'Liu, Yu-Ling'
'Lu, Si-Qi'
'Tang, Yuan-Yuan'
'Chen, Xiao-Gang'
'Gao, Ji-Xing'
'Li, Hao-Jie'
'Xiong, Ren-Gen'
_publ_section_title
;
 Fluorination observed Tc increase of 110 K is challenging
 hydrogen-deuterium isotope effect
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04658E
_journal_year                    2019
_chemical_formula_moiety         'C7 H9 N2, 3(I Pb0.33)'
_chemical_formula_sum            'C7 H9 I3 N2 Pb'
_chemical_formula_weight         709.06
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-17 deposited with the CCDC.    2019-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.6336(7)
_cell_length_b                   10.6336(7)
_cell_length_c                   8.1342(5)
_cell_measurement_reflns_used    735
_cell_measurement_temperature    483(2)
_cell_measurement_theta_max      26.2790
_cell_measurement_theta_min      3.3450
_cell_volume                     796.54(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      483(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2029
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.930
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    16.375
_exptl_absorpt_correction_T_max  0.038
_exptl_absorpt_correction_T_min  0.028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         436
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0406
_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/[σ²(Fo²)+(0.0679P)²+1.2851P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                222
_reflns_number_total             436
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc04658e2.cif
_cod_data_source_block           n-FMDABCO_483K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        796.54(12)
_cod_database_code               7123922
_shelx_shelxl_version_number     2014/7
_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
;

    dai.res created by SHELXL-2014/7


TITL dai in P6(3)/mmc
CELL 0.71073  10.6336  10.6336   8.1342  90.000  90.000 120.000
ZERR    7.00   0.0007   0.0007   0.0005   0.000   0.000   0.000
LATT 1
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM -X, -Y, 0.5+Z
SYMM Y, -X+Y, 0.5+Z
SYMM X-Y, X, 0.5+Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SYMM -Y, -X, 0.5-Z
SYMM -X+Y, Y, 0.5-Z
SYMM X, X-Y, 0.5-Z
SFAC C  H  N  F  I  Pb
UNIT 14 30 4 2 6 2
L.S. 20
ACTA
BOND $H
FMAP 2
PLAN 50
LIST 4
Eqiv $1 1-x+y, 1-x, +z
EQIV $2 1-y, +x-y, +z
EQIV $3 1-y, 1-x, 1/2-z
DFIX 1.5 0.1 C1 C1_$3
SIMU C2 > N1
DELU C2 > N1
SADI N1 C1 N1 C2 N1 C1_$1 C1_$2 N1
SADI C2 C1 C2 C1_$1 C2 C1_$2 C1 C1_$1 C1_$2 C1
TEMP 210.0
WGHT    0.067900    1.285100
FVAR       0.21405
PB1   6    1.000000    1.000000    0.500000    10.08333    0.14754    0.14754 =
         0.08889    0.00000    0.00000    0.07377
I1    5    0.727491    0.863745    0.250000    10.25000    0.14399    0.21265 =
         0.14921    0.00000    0.00000    0.07199
PART  -1
C2    1    0.666633    0.333368    0.548550    10.08333    0.48367    0.48367 =
         0.53350   -0.00875    0.00875    0.14593
AFIX   3
H2A   2    0.715773    0.284228    0.587940    10.08333   -1.50000
H2B   2    0.715773    0.431658    0.587870    10.08333   -1.50000
H2C   2    0.568343    0.284228    0.587860    10.08333   -1.50000
AFIX   0
PART   0
C1    1    0.595921    0.404079    0.323575    10.50000    0.42129    0.42129 =
         0.55648   -0.06259    0.06259    0.26715
AFIX   3
H1A   2    0.644271    0.502120    0.363755    10.50000   -1.20000
AFIX   0
N1    3    0.666667    0.333333    0.378586    10.16667    0.41778    0.41778 =
         0.53381    0.00000    0.00000    0.20889

HKLF 4

REM  dai in P6(3)/mmc
REM R1 =  0.0406 for     222 Fo > 4sig(Fo)  and  0.0690 for all     384 data
REM     25 parameters refined using     32 restraints

END

WGHT      0.0619      1.3112

REM Highest difference peak  0.441,  deepest hole -0.406,  1-sigma level  0.088
Q1    1   1.0000  1.0000  0.6030  10.16667  0.05    0.44
Q2    1   0.7877  0.9588  0.2500  10.50000  0.05    0.37
Q3    1   0.6700  0.8350  0.1675  10.50000  0.05    0.34
Q4    1   0.9539  0.9077  0.4988  10.50000  0.05    0.31
Q5    1   0.7620  0.5240  0.3189  10.50000  0.05    0.31
Q6    1   0.5919  0.4081  0.4830  10.50000  0.05    0.27
Q7    1   1.0000  1.0000  0.2500  10.08333  0.05    0.27
Q8    1   0.6121  0.3879  0.5487  10.50000  0.05    0.23
Q9    1   0.5360  0.4640  0.4413  10.50000  0.05    0.18
Q10   1   0.7292  0.7292  0.5000  10.50000  0.05    0.10
Q11   1   0.8480  0.6960  0.4295  10.50000  0.05    0.09
Q12   1   0.7986  0.8993  0.6129  10.50000  0.05    0.08
Q13   1   0.8382  0.6764  0.3291  10.50000  0.05    0.08
Q14   1   0.6001  0.5224  0.3615  11.00000  0.05    0.08
Q15   1   0.7690  0.8845  0.0034  10.50000  0.05    0.07
Q16   1   0.6202  0.5782  0.3392  11.00000  0.05    0.06
Q17   1   0.8089  0.6178  0.4910  10.50000  0.05    0.06
Q18   1   0.5182  0.4818  0.2500  10.25000  0.05    0.06
Q19   1   0.6600  0.6626  0.3417  11.00000  0.05    0.06
Q20   1   0.7264  0.6620  0.2500  10.50000  0.05    0.05
Q21   1   0.7981  0.7888  0.1153  11.00000  0.05    0.05
Q22   1   1.0565  0.9435  0.6931  10.50000  0.05    0.04
Q23   1   0.4811  0.5189  0.3764  10.50000  0.05    0.03
Q24   1   0.6139  0.5771  0.5421  11.00000  0.05    0.02
Q25   1   0.5916  0.9145  0.2500  10.50000  0.05    0.00
;
_shelx_res_checksum              10343
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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 1.0000 1.0000 0.5000 0.1280(8) Uani 1 12 d S T P . .
I1 I 0.7275(2) 0.86375(10) 0.2500 0.1762(10) Uani 1 4 d S T P . .
C2 C 0.667(2) 0.333(2) 0.549(5) 0.54(6) Uani 0.0833 1 d D U P A -1
H2A H 0.7158 0.2842 0.5879 0.814 Uiso 0.0833 1 d R U P A -1
H2B H 0.7158 0.4317 0.5879 0.814 Uiso 0.0833 1 d R U P A -1
H2C H 0.5683 0.2842 0.5879 0.814 Uiso 0.0833 1 d R U P A -1
C1 C 0.5959(16) 0.4041(16) 0.324(4) 0.44(3) Uani 1 2 d DS TU P A .
H1A H 0.6443 0.5021 0.3638 0.529 Uiso 0.5 1 d R U P . .
N1 N 0.6667 0.3333 0.379(4) 0.46(3) Uani 1 6 d DS TU P . .
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 0.1475(10) 0.1475(10) 0.0889(8) 0.000 0.000 0.0738(5)
I1 0.1440(15) 0.2126(17) 0.1492(15) 0.000 0.000 0.0720(7)
C2 0.48(8) 0.48(8) 0.53(8) -0.01(7) 0.01(7) 0.15(8)
C1 0.42(3) 0.42(3) 0.56(8) -0.063(16) 0.063(16) 0.27(2)
N1 0.42(3) 0.42(3) 0.53(8) 0.000 0.000 0.209(17)
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'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 '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
I1 Pb1 I1 84.57(3) 13_776 14_566
I1 Pb1 I1 95.43(3) 13_776 2_765
I1 Pb1 I1 180.0 14_566 2_765
I1 Pb1 I1 84.57(3) 13_776 15_656
I1 Pb1 I1 84.57(3) 14_566 15_656
I1 Pb1 I1 95.43(3) 2_765 15_656
I1 Pb1 I1 95.43(3) 13_776 3_675
I1 Pb1 I1 95.43(3) 14_566 3_675
I1 Pb1 I1 84.57(3) 2_765 3_675
I1 Pb1 I1 180.0 15_656 3_675
I1 Pb1 I1 180.00(5) 13_776 .
I1 Pb1 I1 95.43(3) 14_566 .
I1 Pb1 I1 84.57(3) 2_765 .
I1 Pb1 I1 95.43(3) 15_656 .
I1 Pb1 I1 84.57(3) 3_675 .
Pb1 I1 Pb1 78.04(4) . 4_774
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C1 N1 109.0(7) 10_665 .
C1 C1 H1A 109.9 10_665 .
N1 C1 H1A 109.9 . .
C1 N1 C1 110.0(7) 2_655 3_665
C1 N1 C1 110.0(7) 2_655 .
C1 N1 C1 110.0(7) 3_665 .
C1 N1 C2 109.0(11) 2_655 .
C1 N1 C2 109.0(11) 3_665 .
C1 N1 C2 108.9(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.2300(14) 13_776
Pb1 I1 3.2300(14) 14_566
Pb1 I1 3.2300(14) 2_765
Pb1 I1 3.2300(14) 15_656
Pb1 I1 3.2300(14) 3_675
Pb1 I1 3.2300(14) .
I1 Pb1 3.2300(14) 4_774
C2 N1 1.38(3) .
C2 H2A 0.9601 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C1 C1 1.20(6) 10_665
C1 N1 1.38(3) .
C1 H1A 0.9602 .
N1 C1 1.38(3) 2_655
N1 C1 1.38(3) 3_665
