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#$Date: 2025-07-06 19:52:23 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300945 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/87/7718705.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_7718705
loop_
_publ_author_name
'Das, Pranjal'
'Kuilya, Hemrupa'
'Basak, Swati'
'Hazarika, Baisali'
'Ray, Joydeep'
'Sarma, Debajit'
'Choudhury, Diganta'
'Kalita, Apurba'
_publ_section_title
;
 Enhancing electrocatalytic water oxidation: ligand complementarity in
 ternary Cu(II) complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9418
_journal_page_last               9426
_journal_paper_doi               10.1039/d5dt00790a
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C4 H12 Br Cu N3, Br'
_chemical_formula_sum            'C4 H12 Br2 Cu N3'
_chemical_formula_weight         325.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-05-13 deposited with the CCDC.	2025-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.702(4)
_cell_length_b                   6.252(3)
_cell_length_c                   8.543(3)
_cell_measurement_reflns_used    3717
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.217
_cell_measurement_theta_min      2.384
_cell_volume                     464.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.217
_diffrn_reflns_theta_max         25.217
_diffrn_reflns_theta_min         2.384
_exptl_absorpt_coefficient_mu    10.883
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_density_diffrn    2.326
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_recrystallization_method 'Slow evaporation in methanol-water'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         497
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0257
_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)+(0.0146P)²+1.9637P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                448
_reflns_number_total             497
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00790a2.cif
_cod_data_source_block           Complex3
_cod_depositor_comments
'Adding full bibliography for 7718704--7718711.cif.'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               7718705
_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_min   0.770
_shelx_estimated_absorpt_t_max   0.804
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
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 0.250000 0.250000 0.66247(9) 0.0247(2) Uani 1 4 d S T P A .
Cu1 Cu 0.250000 0.250000 0.38202(12) 0.0289(3) Uani 1 4 d S T P . .
N2 N 0.250000 0.250000 0.1511(8) 0.0321(19) Uani 1 4 d DS T P A .
C1 C -0.0209(7) 0.250000 0.1946(7) 0.0276(14) Uani 1 2 d DS T P . .
H2B H -0.077426 0.371609 0.153916 0.033 Uiso 0.5 1 calc R U P A .
H2A H -0.090501 0.128797 0.195252 0.033 Uiso 0.5 1 calc R U P . .
Br2 Br 0.250000 0.750000 0.33217(9) 0.0185(2) Uani 1 4 d S T P . .
N1 N 0.0213(6) 0.2961(11) 0.3534(7) 0.023(3) Uani 0.5 1 d D . P A -1
H1A H -0.030509 0.210927 0.418145 0.028 Uiso 0.5 1 calc R U P A -1
H1B H -0.002586 0.430941 0.376257 0.028 Uiso 0.5 1 calc R U P A -1
C2 C 0.1045(7) 0.2026(11) 0.0866(8) 0.019(3) Uani 0.5 1 d D . P A -1
H3A H 0.100978 0.052214 0.058803 0.023 Uiso 0.5 1 calc R U P A -1
H3B H 0.090566 0.285108 -0.008496 0.023 Uiso 0.5 1 calc R U P A -1
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'
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
N2 Cu1 N1 83.08(17) . . ?
N2 Cu1 Br1 180.0 . . ?
N1 Cu1 Br1 96.92(17) . . ?
C2 N2 Cu1 113.0(4) . . ?
N1 C1 C2 116.6(5) . . ?
N1 C1 H2B 108.2 . . ?
C2 C1 H2B 108.2 . . ?
N1 C1 H2A 108.2 . . ?
C2 C1 H2A 108.2 . . ?
H2B C1 H2A 107.3 . . ?
N1 C1 H2B 128.8(3) . 8_565 ?
C2 C1 H2B 89.6(3) . 8_565 ?
H2B C1 H2B 103.2 . 8_565 ?
H2A C1 H2B 22.1 . 8_565 ?
N1 C1 H2A 89.9(3) . 8_565 ?
C2 C1 H2A 129.0(3) . 8_565 ?
H2B C1 H2A 22.1 . 8_565 ?
H2A C1 H2A 102.7 . 8_565 ?
H2B C1 H2A 107.3 8_565 8_565 ?
C1 N1 Cu1 109.7(4) . . ?
C1 N1 H1A 109.7 . . ?
Cu1 N1 H1A 109.7 . . ?
C1 N1 H1B 109.7 . . ?
Cu1 N1 H1B 109.7 . . ?
H1A N1 H1B 108.2 . . ?
N2 C2 C1 112.4(5) . . ?
N2 C2 H3A 109.1 . . ?
C1 C2 H3A 109.1 . . ?
N2 C2 H3B 109.1 . . ?
C1 C2 H3B 109.1 . . ?
H3A C2 H3B 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
Br1 Cu1 2.3959(15) . ?
Cu1 N2 1.972(7) . ?
Cu1 N1 2.026(6) . ?
N2 C2 1.412(6) . ?
C1 N1 1.435(7) . ?
C1 C2 1.460(9) . ?
C1 H2B 0.9700 . ?
C1 H2A 0.9700 . ?
C1 H2B 0.9700 8_565 ?
C1 H2A 0.9700 8_565 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C2 H3A 0.9700 . ?
C2 H3B 0.9700 . ?
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
C2 C1 N1 Cu1 -5.7(5) . . . . ?
Cu1 N2 C2 C1 23.5(5) . . . . ?
N1 C1 C2 N2 -11.3(7) . . . . ?
