#------------------------------------------------------------------------------
#$Date: 2025-03-12 01:37:56 +0200 (Wed, 12 Mar 2025) $
#$Revision: 298387 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/00/7250098.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_7250098
loop_
_publ_author_name
'Zhang, Wanxu'
'Wang, Juan'
'Zheng, Yongzhuo'
'Liu, Mei'
'Wei, Wenqing'
'Guo, Fengwan'
_publ_section_title
;
 Enhancement of intrinsic luminescence by Sb3+ doped (C7H9N)2CdBr6 with
 lone pair 5s2 electrons
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00031A
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'Br4 Cd, 2(C7 H9 Br N)'
_chemical_formula_sum            'C14 H18 Br6 Cd N2'
_chemical_formula_weight         806.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-09 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9533(11)
_cell_length_b                   33.455(4)
_cell_length_c                   8.0313(10)
_cell_measurement_reflns_used    6893
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      3.15
_cell_volume                     2136.9(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27959
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.047
_diffrn_reflns_theta_min         2.632
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.240
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.2610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1825 before and 0.0877 after correction. The Ratio of minimum to maximum transmission is 0.3500. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.462(18)
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0332
_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/[σ²(Fo²)+(0.0289P)²+2.9839P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2451
_reflns_number_total             2856
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00031a2.cif
_cod_data_source_block           x3
_cod_database_code               7250098
_shelx_shelxl_version_number     2019/2
_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_estimated_absorpt_t_max   0.321
_shelx_estimated_absorpt_t_min   0.143
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.538(18)
 0.462(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C4(H4)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_file
;
TITL x3_a.res in Ccc2
    x3.res
    created by SHELXL-2019/2 at 21:20:40 on 18-Nov-2023
REM Old TITL X3 in Ccc2
REM SHELXT solution in Ccc2: R1 0.111, Rweak 0.015, Alpha 0.012
REM <I/s> 0.658 for 101 systematic absences, Orientation as input
REM Flack x = 0.481 ( 0.015 ) from 882 Parsons' quotients
REM Formula found by SHELXT: C10 N4 O2 Br2 In4 Sb
CELL 0.71073 7.9533 33.4548 8.0313 90 90 90
ZERR 4 0.0011 0.0035 0.001 0 0 0
LATT -7
SYMM -X,-Y,+Z
SYMM +X,-Y,0.5+Z
SYMM -X,+Y,0.5+Z
SFAC C H Br Cd N
UNIT 56 72 24 4 8

L.S. 10
PLAN  2
SIZE 0.12 0.23 0.26
TEMP 23
HTAB N1 Br1
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\X3.hkl">
REM </olex2.extras>

WGHT    0.028900    2.983900
EXTI    0.002617
BASF   0.46162
FVAR       0.17374
CD1   4    0.250000    0.750000    0.293673    10.50000    0.02628    0.02852 =
         0.02527    0.00000    0.00000    0.00272
BR2   3    0.490770    0.759867    0.546690    11.00000    0.03110    0.05104 =
         0.03053   -0.00273   -0.01107    0.00160
BR1   3    0.294568    0.671866    0.274218    11.00000    0.03905    0.02743 =
         0.04704   -0.00058   -0.00193    0.00233
BR3   3    0.750770    0.511938    0.767157    11.00000    0.06281    0.05162 =
         0.05419    0.02024    0.00375    0.00577
N1    5    0.718198    0.684478    0.312192    11.00000    0.05130    0.03352 =
         0.04736    0.00415    0.00027    0.00179
AFIX 137
H1A   2    0.725253    0.703590    0.235422    11.00000   -1.20000
H1B   2    0.780508    0.691149    0.399945    11.00000   -1.20000
H1C   2    0.611549    0.681625    0.343573    11.00000   -1.20000
AFIX   0
C5    1    0.759965    0.552738    0.603348    11.00000    0.04784    0.03074 =
         0.02900   -0.00013   -0.00120   -0.00006
C2    1    0.773263    0.612447    0.366170    11.00000    0.05421    0.02438 =
         0.02998   -0.00340    0.00361    0.00006
C3    1    0.621406    0.596127    0.410858    11.00000    0.04776    0.03225 =
         0.04423   -0.00022   -0.00448    0.00954
AFIX  43
H3    2    0.523508    0.605300    0.360359    11.00000   -1.20000
AFIX   0
C6    1    0.913212    0.567866    0.557692    11.00000    0.04253    0.04366 =
         0.03418    0.00537   -0.00010    0.00295
AFIX  43
H6    2    1.011613    0.557937    0.604625    11.00000   -1.20000
AFIX   0
C7    1    0.919258    0.598573    0.439007    11.00000    0.04079    0.04319 =
         0.03715   -0.00496    0.00672   -0.00534
AFIX  43
H7    2    1.022187    0.609654    0.409194    11.00000   -1.20000
AFIX   0
C4    1    0.611376    0.565984    0.530852    11.00000    0.04070    0.03408 =
         0.04387   -0.00252    0.00328   -0.00406
AFIX  43
H4    2    0.508277    0.555099    0.561335    11.00000   -1.20000
AFIX   0
C1    1    0.780556    0.646129    0.241337    11.00000    0.06201    0.04475 =
         0.03775    0.00874    0.00496    0.00017
AFIX  23
H1D   2    0.895761    0.649595    0.204417    11.00000   -1.20000
H1E   2    0.713133    0.639138    0.144998    11.00000   -1.20000
AFIX   0
HKLF 4




REM  x3_a.res in Ccc2
REM wR2 = 0.0750, GooF = S = 1.047, Restrained GooF = 1.046 for all data
REM R1 = 0.0332 for 2451 Fo > 4sig(Fo) and 0.0444 for all 2856 data
REM 108 parameters refined using 1 restraints

END

WGHT      0.0289      2.9901

REM Highest difference peak  0.536,  deepest hole -0.689,  1-sigma level  0.165
Q1    1   0.4240  0.6697  0.2115  11.00000  0.05    0.54
Q2    1   0.2011  0.7703  0.3014  11.00000  0.05    0.53
;
_shelx_res_checksum              51868
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-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
Cd1 Cd 0.250000 0.750000 0.29367(10) 0.02669(16) Uani 1 2 d S T P . .
Br2 Br 0.49077(13) 0.75987(2) 0.54669(10) 0.0376(2) Uani 1 1 d . . . . .
Br1 Br 0.29457(9) 0.67187(2) 0.27422(13) 0.03784(19) Uani 1 1 d . . . . .
Br3 Br 0.75077(10) 0.51194(3) 0.76716(14) 0.0562(3) Uani 1 1 d . . . . .
N1 N 0.7182(8) 0.68448(19) 0.3122(11) 0.0441(18) Uani 1 1 d . . . . .
H1A H 0.725253 0.703590 0.235422 0.053 Uiso 1 1 calc R U . . .
H1B H 0.780508 0.691149 0.399945 0.053 Uiso 1 1 calc R U . . .
H1C H 0.611549 0.681625 0.343573 0.053 Uiso 1 1 calc R U . . .
C5 C 0.7600(10) 0.5527(2) 0.6033(9) 0.0359(16) Uani 1 1 d . . . . .
C2 C 0.7733(10) 0.6124(2) 0.3662(9) 0.0362(17) Uani 1 1 d . . . . .
C3 C 0.6214(11) 0.5961(2) 0.4109(11) 0.0414(18) Uani 1 1 d . . . . .
H3 H 0.523508 0.605300 0.360359 0.050 Uiso 1 1 calc R U . . .
C6 C 0.9132(10) 0.5679(2) 0.5577(11) 0.0401(17) Uani 1 1 d . . . . .
H6 H 1.011613 0.557937 0.604625 0.048 Uiso 1 1 calc R U . . .
C7 C 0.9193(10) 0.5986(3) 0.4390(10) 0.0404(18) Uani 1 1 d . . . . .
H7 H 1.022187 0.609654 0.409194 0.048 Uiso 1 1 calc R U . . .
C4 C 0.6114(10) 0.5660(2) 0.5309(10) 0.0396(19) Uani 1 1 d . . . . .
H4 H 0.508277 0.555099 0.561335 0.047 Uiso 1 1 calc R U . . .
C1 C 0.7806(12) 0.6461(3) 0.2413(11) 0.048(2) Uani 1 1 d . . . . .
H1D H 0.895761 0.649595 0.204417 0.058 Uiso 1 1 calc R U . . .
H1E H 0.713133 0.639138 0.144998 0.058 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
Cd1 0.0263(3) 0.0285(3) 0.0253(3) 0.000 0.000 0.0027(2)
Br2 0.0311(4) 0.0510(4) 0.0305(3) -0.0027(5) -0.0111(3) 0.0016(4)
Br1 0.0391(4) 0.0274(3) 0.0470(4) -0.0006(4) -0.0019(4) 0.0023(2)
Br3 0.0628(5) 0.0516(5) 0.0542(7) 0.0202(5) 0.0038(7) 0.0058(4)
N1 0.051(4) 0.034(3) 0.047(5) 0.004(3) 0.000(4) 0.002(3)
C5 0.048(5) 0.031(4) 0.029(4) 0.000(3) -0.001(3) 0.000(3)
C2 0.054(5) 0.024(3) 0.030(3) -0.003(3) 0.004(3) 0.000(3)
C3 0.048(5) 0.032(4) 0.044(5) 0.000(3) -0.004(4) 0.010(3)
C6 0.043(4) 0.044(4) 0.034(4) 0.005(4) 0.000(4) 0.003(3)
C7 0.041(4) 0.043(4) 0.037(4) -0.005(3) 0.007(3) -0.005(3)
C4 0.041(4) 0.034(4) 0.044(5) -0.003(3) 0.003(4) -0.004(3)
C1 0.062(5) 0.045(4) 0.038(5) 0.009(4) 0.005(4) 0.000(4)
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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
Br2 Cd1 Br2 87.44(5) . 6_565 ?
Br2 Cd1 Br2 92.94(5) 7_464 4_654 ?
Br2 Cd1 Br2 89.814(11) . 4_654 ?
Br2 Cd1 Br2 89.814(11) 6_565 7_464 ?
Br2 Cd1 Br2 177.21(5) . 7_464 ?
Br2 Cd1 Br2 177.21(5) 6_565 4_654 ?
Br1 Cd1 Br2 86.67(3) 6_565 4_654 ?
Br1 Cd1 Br2 86.67(3) . 7_464 ?
Br1 Cd1 Br2 93.87(3) 6_565 6_565 ?
Br1 Cd1 Br2 91.03(3) 6_565 . ?
Br1 Cd1 Br2 88.66(3) 6_565 7_464 ?
Br1 Cd1 Br2 88.66(3) . 4_654 ?
Br1 Cd1 Br2 91.03(3) . 6_565 ?
Br1 Cd1 Br2 93.87(3) . . ?
Br1 Cd1 Br1 173.22(6) . 6_565 ?
Cd1 Br2 Cd1 166.39(3) . 7_565 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C6 C5 Br3 119.1(6) . . ?
C6 C5 C4 121.8(7) . . ?
C4 C5 Br3 119.1(6) . . ?
C3 C2 C7 119.7(7) . . ?
C3 C2 C1 120.3(8) . . ?
C7 C2 C1 120.0(7) . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.2(8) . . ?
C4 C3 H3 119.4 . . ?
C5 C6 H6 120.6 . . ?
C5 C6 C7 118.9(8) . . ?
C7 C6 H6 120.6 . . ?
C2 C7 C6 120.4(7) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C5 C4 C3 118.1(7) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N1 C1 C2 112.1(8) . . ?
N1 C1 H1D 109.2 . . ?
N1 C1 H1E 109.2 . . ?
C2 C1 H1D 109.2 . . ?
C2 C1 H1E 109.2 . . ?
H1D C1 H1E 107.9 . . ?
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 Br2 2.8116(11) . ?
Cd1 Br2 2.8800(11) 4_654 ?
Cd1 Br2 2.8800(11) 7_464 ?
Cd1 Br2 2.8116(11) 6_565 ?
Cd1 Br1 2.6425(7) . ?
Cd1 Br1 2.6426(7) 6_565 ?
Br3 C5 1.897(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.489(11) . ?
C5 C6 1.370(11) . ?
C5 C4 1.390(11) . ?
C2 C3 1.373(12) . ?
C2 C7 1.381(11) . ?
C2 C1 1.509(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.397(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.402(11) . ?
C7 H7 0.9300 . ?
C4 H4 0.9300 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
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 H1C Br1 0.89 2.60 3.409(7) 151.2 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br3 C5 C6 C7 -178.7(6) . . . . ?
Br3 C5 C4 C3 179.8(6) . . . . ?
C5 C6 C7 C2 -1.8(12) . . . . ?
C2 C3 C4 C5 -0.4(12) . . . . ?
C3 C2 C7 C6 0.2(12) . . . . ?
C3 C2 C1 N1 72.5(10) . . . . ?
C6 C5 C4 C3 -1.3(12) . . . . ?
C7 C2 C3 C4 0.9(12) . . . . ?
C7 C2 C1 N1 -105.9(9) . . . . ?
C4 C5 C6 C7 2.4(12) . . . . ?
C1 C2 C3 C4 -177.5(8) . . . . ?
C1 C2 C7 C6 178.7(8) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.538(18)
2 0.462(18)
