#------------------------------------------------------------------------------
#$Date: 2025-07-10 14:18:13 +0300 (Thu, 10 Jul 2025) $
#$Revision: 301209 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/90/1569005.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_1569005
loop_
_publ_author_name
'Zhou, Shuigen'
'Chen, Yihao'
'Li, Kailei'
'Liu, Xiaowei'
'Zhang, Ting'
'Shen, Wei'
'Li, Ming'
'Zhou, Lei'
'He, Rongxing'
_publ_section_title
;
 Photophysical studies for Cu(i)-based halides: broad excitation bands and
 highly efficient single-component warm white-light-emitting diodes.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              5415
_journal_page_last               5424
_journal_paper_doi               10.1039/d3sc01762a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'Br6 Cu4, 6(H2 O2 P), 4(C6 H10 N2)'
_chemical_formula_sum            'C24 H52 Br6 Cu4 N8 O12 P6'
_chemical_formula_weight         1564.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-01-15 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6690(6)
_cell_length_b                   13.6690(6)
_cell_length_c                   51.320(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.98
_cell_volume                     9588.7(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX3 V2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_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      173.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE TXS PHOTON 100'
_diffrn_measurement_method       'ω and φ shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            40139
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.252
_diffrn_source                   TXS
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Rotaing Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.011
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1324 before and 0.0974 after correction.
The Ratio of minimum to maximum transmission is 0.5833.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    2.167
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0323
_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)+(0.0293P)²+58.3632P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2346
_reflns_number_total             2759
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01762a2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1569003--1569005.cif.

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H26 Br3 Cu2 N4 O6 P3'
_cod_original_formula_weight         782.09
_cod_original_formula_moiety         '0.5(Br6 Cu4), 3(H2 O2 P), 2(C6 H10 N2)'
_cod_original_formula_units_Z            16
_cod_original_cell_volume        9588.8(11)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               1569005
_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   0.541
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
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
Br1 Br 0.72277(2) 0.73677(3) 0.37545(2) 0.01949(11) Uani 1 1 d . . . . .
Br2 Br 0.500000 0.750000 0.42901(2) 0.01634(12) Uani 1 2 d S T P . .
Cu1 Cu 0.57456(3) 0.66483(4) 0.39191(2) 0.02734(14) Uani 1 1 d . . . . .
P1 P 1.000000 0.750000 0.41480(2) 0.0213(3) Uani 1 2 d S T P . .
H1 H 0.946(3) 0.802(3) 0.3986(9) 0.038(13) Uiso 1 1 d . . . . .
O1 O 0.93705(18) 0.68054(18) 0.43003(5) 0.0239(5) Uani 1 1 d . . . . .
P2 P 0.73255(7) 0.48512(7) 0.41651(2) 0.0204(2) Uani 1 1 d . . . . .
H2D H 0.798(3) 0.532(3) 0.4012(8) 0.037(13) Uiso 1 1 d . . . . .
H2E H 0.680(3) 0.436(3) 0.4005(8) 0.037(12) Uiso 1 1 d . . . . .
O2 O 0.78610(18) 0.42238(18) 0.43590(5) 0.0212(5) Uani 1 1 d . . . . .
O3 O 0.66054(17) 0.55842(18) 0.42717(5) 0.0205(5) Uani 1 1 d . . . . .
N1 N 0.7494(2) 0.7286(2) 0.44486(5) 0.0154(5) Uani 1 1 d . . . . .
H1A H 0.705829 0.683749 0.438740 0.018 Uiso 1 1 calc R U . . .
H1B H 0.810237 0.714044 0.438812 0.018 Uiso 1 1 calc R U . . .
H1C H 0.731798 0.789295 0.439307 0.018 Uiso 1 1 calc R U . . .
C1 C 0.7497(3) 0.7263(2) 0.47335(6) 0.0159(6) Uani 1 1 d . . . . .
C2 C 0.8355(3) 0.7254(5) 0.48635(8) 0.0494(14) Uani 1 1 d . . . . .
H2 H 0.895522 0.724700 0.477031 0.059 Uiso 1 1 calc R U . . .
C3 C 0.8356(3) 0.7254(5) 0.51353(8) 0.0529(15) Uani 1 1 d . . . . .
H3 H 0.895777 0.724783 0.522782 0.063 Uiso 1 1 calc R U . . .
N2 N 0.4768(2) 0.5062(2) 0.44515(5) 0.0175(6) Uani 1 1 d . . . . .
H2A H 0.532180 0.530326 0.437694 0.021 Uiso 1 1 calc R U . . .
H2B H 0.425193 0.545160 0.440987 0.021 Uiso 1 1 calc R U . . .
H2C H 0.465681 0.444498 0.439163 0.021 Uiso 1 1 calc R U . . .
C4 C 0.4888(2) 0.5037(3) 0.47345(6) 0.0162(6) Uani 1 1 d . . . . .
C5 C 0.5771(3) 0.4762(4) 0.48385(7) 0.0431(13) Uani 1 1 d . . . . .
H5 H 0.630303 0.459819 0.472771 0.052 Uiso 1 1 calc R U . . .
C6 C 0.5878(3) 0.4725(4) 0.51084(7) 0.0416(12) Uani 1 1 d . . . . .
H6 H 0.648567 0.453441 0.518262 0.050 Uiso 1 1 calc R U . . .
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'
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
Cu1 Br1 Cu1 71.03(3) 28_656 . ?
Cu1 Br2 Cu1 78.19(3) . 10_564 ?
Br1 Cu1 Br1 127.64(2) 19_576 . ?
Br1 Cu1 Br2 115.368(19) . . ?
Br1 Cu1 Br2 116.858(19) 19_576 . ?
Br1 Cu1 Cu1 54.53(2) 19_576 19_576 ?
Br1 Cu1 Cu1 114.78(2) . 19_576 ?
Br1 Cu1 Cu1 114.05(2) 19_576 28_656 ?
Br1 Cu1 Cu1 54.44(2) . 28_656 ?
Br2 Cu1 Cu1 97.635(18) . 19_576 ?
Br2 Cu1 Cu1 97.634(18) . 28_656 ?
Cu1 Cu1 Cu1 67.289(18) 19_576 28_656 ?
H1 P1 H1 102(4) . 10_664 ?
O1 P1 H1 110.2(19) . . ?
O1 P1 H1 108.0(19) 10_664 . ?
O1 P1 H1 110.2(19) 10_664 10_664 ?
O1 P1 H1 108.0(19) . 10_664 ?
O1 P1 O1 117.2(2) . 10_664 ?
H2D P2 H2E 104(3) . . ?
O2 P2 H2D 109.5(19) . . ?
O2 P2 H2E 113(2) . . ?
O2 P2 O3 117.19(14) . . ?
O3 P2 H2D 109.0(18) . . ?
O3 P2 H2E 102.7(19) . . ?
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 . . ?
C2 C1 N1 119.8(3) . . ?
C3 C1 N1 119.8(3) 5_656 . ?
C3 C1 C2 120.4(3) 5_656 . ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C3 C2 119.9(4) 5_656 . ?
C1 C3 H3 120.0 5_656 . ?
C2 C3 H3 120.0 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C5 C4 N2 119.4(3) . . ?
C6 C4 N2 119.8(3) 17_666 . ?
C6 C4 C5 120.8(3) 17_666 . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.3(4) . . ?
C6 C5 H5 120.4 . . ?
C4 C6 C5 119.9(4) 17_666 . ?
C4 C6 H6 120.0 17_666 . ?
C5 C6 H6 120.0 . . ?
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
Br1 Cu1 2.4025(6) 28_656 ?
Br1 Cu1 2.4050(6) . ?
Br2 Cu1 2.4538(6) 10_564 ?
Br2 Cu1 2.4536(6) . ?
Cu1 Cu1 2.7927(9) 28_656 ?
Cu1 Cu1 2.7927(9) 19_576 ?
P1 H1 1.32(5) 10_664 ?
P1 H1 1.32(5) . ?
P1 O1 1.501(3) 10_664 ?
P1 O1 1.501(3) . ?
P2 H2D 1.35(5) . ?
P2 H2E 1.28(5) . ?
P2 O2 1.504(2) . ?
P2 O3 1.507(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.463(4) . ?
C1 C2 1.348(5) . ?
C1 C3 1.347(5) 5_656 ?
C2 H2 0.9500 . ?
C2 C3 1.395(5) . ?
C3 H3 0.9500 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C4 1.462(4) . ?
C4 C5 1.372(5) . ?
C4 C6 1.361(5) 17_666 ?
C5 H5 0.9500 . ?
C5 C6 1.394(5) . ?
C6 H6 0.9500 . ?
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
N1 C1 C2 C3 178.6(5) . . . . ?
C1 C2 C3 C1 0.0(9) . . . 5_656 ?
C3 C1 C2 C3 -1.3(7) 5_656 . . . ?
N2 C4 C5 C6 -179.0(4) . . . . ?
C4 C5 C6 C4 -0.1(8) . . . 17_666 ?
C6 C4 C5 C6 0.1(9) 17_666 . . . ?
