#------------------------------------------------------------------------------
#$Date: 2025-07-10 14:18:13 +0300 (Thu, 10 Jul 2025) $
#$Revision: 301209 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/90/1569003.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_1569003
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         'Cl6 Cu4, 6(H2 O2 P), 4(C6 H10 N2)'
_chemical_formula_sum            'C24 H52 Cl6 Cu4 N8 O12 P6'
_chemical_formula_weight         1297.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :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            4
_cell_length_a                   13.6165(6)
_cell_length_b                   25.2859(10)
_cell_length_c                   13.6152(5)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.99
_cell_volume                     4687.8(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21079
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.992
_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    2.398
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1095 before and 0.0535 after correction.
The Ratio of minimum to maximum transmission is 0.6359.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0271
_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)+(0.0232P)²+10.2149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2415
_reflns_number_total             2696
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01762a2.cif
_cod_data_source_block           a
_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 Cl3 Cu2 N4 O6 P3'
_cod_original_formula_weight         648.71
_cod_original_formula_moiety         '0.5(Cl6 Cu4), 3(H2 O2 P), 2(C6 H10 N2)'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1569003
_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   0.795
_shelx_estimated_absorpt_t_min   0.762
_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:
 C1(H1), 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'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, 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
Cu1 Cu 0.92302(2) 0.28440(2) 0.32820(2) 0.03560(9) Uani 1 1 d . . . . .
Cl1 Cl 0.78883(5) 0.250000 0.250000 0.03118(16) Uani 1 2 d S T P . .
Cl2 Cl 1.000000 0.250000 0.46297(5) 0.03398(17) Uani 1 2 d S T P . .
Cl3 Cl 1.000000 0.35697(3) 0.250000 0.02611(14) Uani 1 2 d S T P . .
P1 P 0.76637(4) 0.33040(2) 0.51332(4) 0.02517(12) Uani 1 1 d . . . . .
H1D H 0.8159(18) 0.2976(10) 0.5690(17) 0.036(6) Uiso 1 1 d . . . . .
H1E H 0.702(2) 0.2992(11) 0.4685(19) 0.047(7) Uiso 1 1 d . . . . .
O1 O 0.83656(10) 0.35191(6) 0.43780(10) 0.0286(3) Uani 1 1 d . . . . .
O2 O 0.71377(11) 0.37010(6) 0.57641(10) 0.0306(3) Uani 1 1 d . . . . .
P2 P 0.500000 0.32598(3) 0.250000 0.02674(16) Uani 1 2 d S T P . .
H2 H 0.4389(17) 0.2936(10) 0.3017(18) 0.035(7) Uiso 1 1 d . . . . .
O3 O 0.56140(12) 0.35693(7) 0.32082(11) 0.0373(4) Uani 1 1 d . . . . .
N1 N 0.74941(13) 0.38811(6) 0.26933(11) 0.0248(3) Uani 1 1 d . . . . .
H1A H 0.769800 0.376782 0.209253 0.030 Uiso 1 1 calc R U . . .
H1B H 0.687569 0.376002 0.280997 0.030 Uiso 1 1 calc R U . . .
H1C H 0.790824 0.375562 0.316329 0.030 Uiso 1 1 calc R U . . .
C1 C 0.83703(17) 0.47253(9) 0.2728(2) 0.0429(6) Uani 1 1 d . . . . .
H1 H 0.897253 0.453573 0.273819 0.051 Uiso 1 1 calc R U . . .
C2 C 0.74949(15) 0.44566(8) 0.27158(13) 0.0236(4) Uani 1 1 d . . . . .
C3 C 0.66243(17) 0.47290(9) 0.2726(2) 0.0418(6) Uani 1 1 d . . . . .
H3 H 0.601879 0.454240 0.273264 0.050 Uiso 1 1 calc R U . . .
N2 N 0.52138(12) 0.38852(6) 0.50899(12) 0.0244(3) Uani 1 1 d . . . . .
H2A H 0.531016 0.375761 0.447237 0.029 Uiso 1 1 calc R U . . .
H2B H 0.466114 0.373866 0.534914 0.029 Uiso 1 1 calc R U . . .
H2C H 0.573917 0.380154 0.547262 0.029 Uiso 1 1 calc R U . . .
C4 C 0.51028(15) 0.44592(8) 0.50505(14) 0.0237(4) Uani 1 1 d . . . . .
C5 C 0.42175(17) 0.46753(9) 0.4782(2) 0.0414(6) Uani 1 1 d . . . . .
H5 H 0.367713 0.445201 0.463098 0.050 Uiso 1 1 calc R U . . .
C6 C 0.41140(17) 0.52194(9) 0.4733(2) 0.0402(6) Uani 1 1 d . . . . .
H6 H 0.350192 0.537012 0.454857 0.048 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'
Cl Cl 0.1484 0.1585 '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 Cu1 Cu1 56.504(11) 8_455 3_755 ?
Cu1 Cu1 Cu1 57.326(12) 6_655 3_755 ?
Cu1 Cu1 Cu1 66.172(12) 6_655 8_455 ?
Cl1 Cu1 Cu1 103.224(17) . 3_755 ?
Cl1 Cu1 Cu1 111.839(17) . 6_655 ?
Cl1 Cu1 Cu1 53.040(13) . 8_455 ?
Cl1 Cu1 Cl3 116.066(12) . . ?
Cl2 Cu1 Cu1 53.413(13) . 6_655 ?
Cl2 Cu1 Cu1 112.398(17) . 8_455 ?
Cl2 Cu1 Cu1 104.503(17) . 3_755 ?
Cl2 Cu1 Cl1 126.556(13) . . ?
Cl2 Cu1 Cl3 116.954(12) . . ?
Cl3 Cu1 Cu1 98.171(16) . 8_455 ?
Cl3 Cu1 Cu1 50.846(12) . 3_755 ?
Cl3 Cu1 Cu1 98.878(17) . 6_655 ?
Cu1 Cl1 Cu1 73.92(3) . 8_455 ?
Cu1 Cl2 Cu1 73.17(3) 6_655 . ?
Cu1 Cl3 Cu1 78.31(2) 3_755 . ?
H1D P1 H1E 103.1(15) . . ?
O1 P1 H1D 107.3(11) . . ?
O1 P1 H1E 108.6(11) . . ?
O2 P1 H1D 109.7(10) . . ?
O2 P1 H1E 110.4(12) . . ?
O2 P1 O1 116.86(9) . . ?
O3 P2 H2 108.8(10) . . ?
O3 P2 H2 107.8(10) 3_655 . ?
O3 P2 O3 116.96(14) . 3_655 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
C2 C1 H1 120.0 . . ?
C2 C1 C3 120.0(2) . 2_665 ?
C3 C1 H1 120.0 2_665 . ?
C1 C2 N1 119.73(18) . . ?
C3 C2 N1 120.12(19) . . ?
C3 C2 C1 120.15(19) . . ?
C1 C3 H3 120.1 2_665 . ?
C2 C3 C1 119.8(2) . 2_665 ?
C2 C3 H3 120.1 . . ?
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 119.75(19) . . ?
C6 C4 N2 120.01(18) 9_666 . ?
C6 C4 C5 120.24(19) 9_666 . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.9(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C6 C5 119.9(2) 9_666 . ?
C4 C6 H6 120.0 9_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
Cu1 Cu1 2.7241(6) 6_655 ?
Cu1 Cu1 2.9882(6) 3_755 ?
Cu1 Cu1 2.7497(6) 8_455 ?
Cu1 Cl1 2.2867(6) . ?
Cu1 Cl2 2.2852(6) . ?
Cu1 Cl3 2.3663(6) . ?
P1 H1D 1.31(2) . ?
P1 H1E 1.32(3) . ?
P1 O1 1.5054(14) . ?
P1 O2 1.5027(14) . ?
P2 H2 1.36(2) . ?
P2 O3 1.4971(16) . ?
P2 O3 1.4971(16) 3_655 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C2 1.456(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.372(3) . ?
C1 C3 1.380(3) 2_665 ?
C2 C3 1.371(3) . ?
C3 H3 0.9500 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C4 1.460(2) . ?
C4 C5 1.373(3) . ?
C4 C6 1.373(3) 9_666 ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
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 C2 C3 C1 -178.7(2) . . . 2_665 ?
C1 C2 C3 C1 1.4(3) . . . 2_665 ?
C3 C1 C2 N1 178.5(2) 2_665 . . . ?
C3 C1 C2 C3 -1.6(3) 2_665 . . . ?
N2 C4 C5 C6 -179.2(2) . . . . ?
C4 C5 C6 C4 0.1(4) . . . 9_666 ?
C6 C4 C5 C6 -0.1(4) 9_666 . . . ?
