#------------------------------------------------------------------------------
#$Date: 2025-04-11 01:11:14 +0300 (Fri, 11 Apr 2025) $
#$Revision: 299256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/43/1574382.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_1574382
loop_
_publ_author_name
'Cui, Yibo'
'Lin, Jiawei'
'Liu, Kunjie'
'Shao, Yuhe'
'Zhao, Dong'
'Guo, Zhongnan'
'Zhao, Jing'
'Xia, Zhiguo'
'Liu, Quanlin'
_publ_section_title
;
 Tuning Covalent Bonding in Znic-Based Hybrid Halides towards Tunable
 Room-Temperature Phosphorescence
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC00931F
_journal_year                    2025
_chemical_formula_moiety         'Br4 Zn, 2(C6 H9 N2)'
_chemical_formula_sum            'C12 H18 Br4 N4 Zn'
_chemical_formula_weight         603.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-12-30 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.194(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4961(6)
_cell_length_b                   7.8886(4)
_cell_length_c                   16.3790(8)
_cell_measurement_reflns_used    5127
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.389
_cell_measurement_theta_min      2.491
_cell_volume                     1870.09(15)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13958
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         2.491
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.858
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1393 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.2681. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'dull whiteish white'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0219
_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)+(0.0287P)²+0.1102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1582
_reflns_number_total             1926
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL mo_1128_4_0m_a.res in C2/c
    mo_1128_4_0m.res
    created by SHELXL-2018/3 at 15:51:31 on 30-Dec-2024
REM Old TITL mo_1128_4_0m_a.res in C2/c
REM SHELXT solution in C2/c: R1 0.072, Rweak 0.002, Alpha 0.017
REM <I/s> 0.843 for 143 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 Br4 N4 Zn
CELL 0.71073 14.4961 7.8886 16.379 90 93.194 90
ZERR 4 0.0006 0.0004 0.0008 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br N Zn
UNIT 48 72 16 16 4

L.S. 60
PLAN  5
TEMP -123.15
BOND
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\mo_1128_4_0m.hkl">
REM </olex2.extras>

WGHT    0.028700    0.110200
FVAR       0.23253
BR2   3    0.562065    0.414151    0.642416    11.00000    0.03615    0.03596 =
         0.03780   -0.00493    0.00792   -0.00180
BR4   3    0.616791    0.758724    0.818395    11.00000    0.03278    0.04372 =
         0.04137   -0.00620    0.00232   -0.00413
ZN1   5    0.500000    0.588932    0.750000    10.50000    0.03124    0.03236 =
         0.03309    0.00000    0.00367    0.00000
N2    4    0.395070    0.179811    0.535295    11.00000    0.03520    0.03491 =
         0.03853   -0.00082   -0.00198    0.00071
AFIX  43
H2    2    0.421106    0.245420    0.573440    11.00000   -1.20000
AFIX   0
N1    4    0.275069    0.131666    0.620373    11.00000    0.03459    0.04337 =
         0.04441    0.00056    0.00562   -0.00221
AFIX  43
H1    2    0.219276    0.091246    0.626394    11.00000   -1.20000
AFIX   0
C2    1    0.314083    0.102188    0.550509    11.00000    0.03612    0.03360 =
         0.03397    0.00476    0.00553    0.00724
C6    1    0.437457    0.161230    0.464653    11.00000    0.03923    0.03971 =
         0.03640    0.00268    0.00431    0.00354
AFIX  43
H6    2    0.493280    0.220532    0.456684    11.00000   -1.20000
AFIX   0
C4    1    0.318958   -0.026192    0.418518    11.00000    0.04611    0.03866 =
         0.03899   -0.00088   -0.00404    0.00353
AFIX  43
H4    2    0.293163   -0.099554    0.377294    11.00000   -1.20000
AFIX   0
C3    1    0.275330   -0.006394    0.488896    11.00000    0.03544    0.03404 =
         0.04913    0.00668    0.00022    0.00260
AFIX  43
H3    2    0.219235   -0.064833    0.496846    11.00000   -1.20000
AFIX   0
C5    1    0.401262    0.059408    0.405473    11.00000    0.04421    0.04294 =
         0.03609    0.00449    0.00128    0.00541
AFIX  43
H5    2    0.431042    0.045812    0.355671    11.00000   -1.20000
AFIX   0
C1    1    0.319367    0.227153    0.687671    11.00000    0.04177    0.04753 =
         0.04168   -0.00273    0.00575   -0.00091
AFIX 137
H1A   2    0.332898    0.342216    0.669211    11.00000   -1.50000
H1B   2    0.377052    0.170864    0.706221    11.00000   -1.50000
H1C   2    0.277997    0.232709    0.732921    11.00000   -1.50000
AFIX   0
HKLF 4




REM  mo_1128_4_0m_a.res in C2/c
REM wR2 = 0.0533, GooF = S = 1.038, Restrained GooF = 1.038 for all data
REM R1 = 0.0219 for 1582 Fo > 4sig(Fo) and 0.0324 for all 1926 data
REM 97 parameters refined using 0 restraints

END  
     
WGHT      0.0287      0.1102 

REM Highest difference peak  0.348,  deepest hole -0.417,  1-sigma level  0.073
Q1    1   0.5621  0.2995  0.6452  11.00000  0.05    0.35
Q2    1   0.6191  0.4762  0.6543  11.00000  0.05    0.33
Q3    1   0.5855  0.8590  0.8193  11.00000  0.05    0.30
Q4    1   0.3611  0.2067  0.6298  11.00000  0.05    0.30
Q5    1   0.6095  0.6434  0.8180  11.00000  0.05    0.30

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0219 for 1582 Fo > 4sig(Fo) and 0.0324 for all 14563 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.35, deepest hole -0.42
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0324
  REM R1_gt = 0.0219
  REM wR_ref = 0.0533
  REM GOOF = 1.038
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 14563
  REM Reflections_gt = 1582
  REM Parameters = n/a
  REM Hole = -0.42
  REM Peak = 0.35
  REM Flack = n/a

  
;
_cod_data_source_file            d5sc00931f2.cif
_cod_data_source_block           mo_1128_4_0m
_cod_database_code               1574382
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C6(H6), C4(H4), C3(H3), C5(H5)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Br2 Br 0.56207(2) 0.41415(4) 0.64242(2) 0.03642(10) Uani 1 1 d . . . . .
Br4 Br 0.61679(2) 0.75872(4) 0.81840(2) 0.03928(10) Uani 1 1 d . . . . .
Zn1 Zn 0.500000 0.58893(6) 0.750000 0.03216(12) Uani 1 2 d S T P . .
N2 N 0.39507(16) 0.1798(3) 0.53529(16) 0.0364(6) Uani 1 1 d . . . . .
H2 H 0.421106 0.245420 0.573440 0.044 Uiso 1 1 calc R . . . .
N1 N 0.27507(17) 0.1317(3) 0.62037(16) 0.0407(6) Uani 1 1 d . . . . .
H1 H 0.219276 0.091246 0.626394 0.049 Uiso 1 1 calc R . . . .
C2 C 0.31408(19) 0.1022(3) 0.55051(19) 0.0344(6) Uani 1 1 d . . . . .
C6 C 0.4375(2) 0.1612(4) 0.46465(19) 0.0384(7) Uani 1 1 d . . . . .
H6 H 0.493280 0.220532 0.456684 0.046 Uiso 1 1 calc R . . . .
C4 C 0.3190(2) -0.0262(4) 0.4185(2) 0.0415(7) Uani 1 1 d . . . . .
H4 H 0.293163 -0.099554 0.377294 0.050 Uiso 1 1 calc R . . . .
C3 C 0.2753(2) -0.0064(4) 0.4889(2) 0.0396(7) Uani 1 1 d . . . . .
H3 H 0.219235 -0.064833 0.496846 0.048 Uiso 1 1 calc R . . . .
C5 C 0.4013(2) 0.0594(4) 0.4055(2) 0.0411(7) Uani 1 1 d . . . . .
H5 H 0.431042 0.045812 0.355671 0.049 Uiso 1 1 calc R . . . .
C1 C 0.3194(2) 0.2272(4) 0.6877(2) 0.0435(7) Uani 1 1 d . . . . .
H1A H 0.332898 0.342216 0.669211 0.065 Uiso 1 1 calc GR . . . .
H1B H 0.377052 0.170864 0.706221 0.065 Uiso 1 1 calc GR . . . .
H1C H 0.277997 0.232709 0.732921 0.065 Uiso 1 1 calc GR . . . .
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
Br2 0.03615(16) 0.03596(16) 0.03780(18) -0.00493(13) 0.00792(12) -0.00180(12)
Br4 0.03278(15) 0.04372(18) 0.04137(19) -0.00620(14) 0.00232(12) -0.00413(12)
Zn1 0.0312(2) 0.0324(2) 0.0331(3) 0.000 0.00367(18) 0.000
N2 0.0352(12) 0.0349(13) 0.0385(15) -0.0008(11) -0.0020(11) 0.0007(10)
N1 0.0346(13) 0.0434(14) 0.0444(17) 0.0006(12) 0.0056(11) -0.0022(11)
C2 0.0361(14) 0.0336(15) 0.0340(16) 0.0048(12) 0.0055(12) 0.0072(11)
C6 0.0392(15) 0.0397(16) 0.0364(18) 0.0027(14) 0.0043(13) 0.0035(13)
C4 0.0461(17) 0.0387(16) 0.0390(19) -0.0009(14) -0.0040(14) 0.0035(13)
C3 0.0354(15) 0.0340(15) 0.049(2) 0.0067(14) 0.0002(13) 0.0026(12)
C5 0.0442(16) 0.0429(17) 0.0361(18) 0.0045(14) 0.0013(13) 0.0054(14)
C1 0.0418(16) 0.0475(18) 0.0417(19) -0.0027(15) 0.0058(14) -0.0009(13)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 Zn1 Br2 111.44(2) . 2_656 ?
Br4 Zn1 Br2 111.972(10) 2_656 2_656 ?
Br4 Zn1 Br2 111.973(10) . . ?
Br4 Zn1 Br2 104.928(11) 2_656 . ?
Br4 Zn1 Br2 104.928(11) . 2_656 ?
Br4 Zn1 Br4 111.77(2) . 2_656 ?
C6 N2 C2 123.2(3) . . ?
C2 N1 C1 123.6(3) . . ?
N2 C2 C3 117.0(3) . . ?
N1 C2 N2 119.6(3) . . ?
N1 C2 C3 123.4(3) . . ?
C5 C6 N2 120.4(3) . . ?
C3 C4 C5 121.2(3) . . ?
C4 C3 C2 119.4(3) . . ?
C6 C5 C4 118.8(3) . . ?
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
Br2 Zn1 2.4479(4) . ?
Br4 Zn1 2.3883(4) . ?
N2 C2 1.359(4) . ?
N2 C6 1.348(4) . ?
N1 C2 1.325(4) . ?
N1 C1 1.455(4) . ?
C2 C3 1.416(4) . ?
C6 C5 1.343(4) . ?
C4 C3 1.354(4) . ?
C4 C5 1.398(4) . ?
