#------------------------------------------------------------------------------
#$Date: 2023-01-04 03:13:08 +0100 (Wed 04 de Jan de 2023) $
#$Revision: 280092 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/60/7246072.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_7246072
loop_
_publ_author_name
'Cáceres-Vásquez, Joaquín'
'Jara, Danilo H.'
'Costamagna, Juan'
'Martínez-Gómez, Fabián'
'Silva, Carlos P.'
'Lemus, Luis'
'Freire, Eleonora'
'Baggio, Ricardo'
'Vera, Cristian'
'Guerrero, Juan'
_publ_section_title
;
 Effect of non-covalent self-dimerization on the spectroscopic and
 electrochemical properties of mixed Cu(i) complexes
;
_journal_issue                   2
_journal_name_full               'RSC Advances'
_journal_page_first              825
_journal_page_last               838
_journal_paper_doi               10.1039/D2RA05341A
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C30 H24 Br Cu N3 O2 P'
_chemical_formula_sum            'C30 H24 Br Cu N3 O2 P'
_chemical_formula_weight         632.94
_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
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-06-28 deposited with the CCDC.	2022-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.499(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.966(2)
_cell_length_b                   9.1945(4)
_cell_length_c                   20.1441(13)
_cell_measurement_reflns_used    3244
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.432
_cell_measurement_theta_min      3.782
_cell_volume                     5580.2(7)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0604
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            9502
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.178
_diffrn_reflns_theta_min         3.753
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Oxford Diffraction, 2009)'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.78
_exptl_transmission_factor_min   0.60
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5845
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0436
_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)+(0.0563P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3091
_reflns_number_total             5845
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra05341a2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7246072
_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.
;
_shelxl_version_number           2014/6
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
Cu1 Cu 0.40097(2) 0.38758(6) -0.02797(3) 0.04590(16) Uani 1 1 d . U . . .
Br1 Br 0.40795(2) 0.25938(5) -0.12700(2) 0.05660(16) Uani 1 1 d . U . . .
P1 P 0.34317(3) 0.32786(12) -0.01248(5) 0.0374(3) Uani 1 1 d . U . . .
N1 N 0.40944(10) 0.6089(4) -0.04289(18) 0.0473(8) Uani 1 1 d . U . . .
N2 N 0.46531(10) 0.4236(4) 0.06007(17) 0.0457(8) Uani 1 1 d . U . . .
N3 N 0.56917(19) -0.0189(6) 0.2563(3) 0.0939(15) Uani 1 1 d . U . . .
O1 O 0.55106(15) -0.1277(5) 0.2575(3) 0.1188(15) Uani 1 1 d . U . . .
O2 O 0.61043(15) 0.0004(5) 0.2865(2) 0.1244(15) Uani 1 1 d . U . . .
C11 C 0.32970(12) 0.1350(4) -0.0164(2) 0.0385(8) Uani 1 1 d . U . . .
C21 C 0.35969(13) 0.0443(5) 0.0388(2) 0.0527(11) Uani 1 1 d . U . . .
H21 H 0.3855 0.0837 0.0768 0.063 Uiso 1 1 calc R U . . .
C31 C 0.35200(16) -0.1030(5) 0.0385(3) 0.0660(13) Uani 1 1 d . U . . .
H31 H 0.3726 -0.1622 0.0757 0.079 Uiso 1 1 calc R U . . .
C41 C 0.31403(16) -0.1617(5) -0.0166(3) 0.0672(12) Uani 1 1 d . U . . .
H41 H 0.3087 -0.2610 -0.0168 0.081 Uiso 1 1 calc R U . . .
C51 C 0.28367(16) -0.0741(5) -0.0717(3) 0.0701(13) Uani 1 1 d . U . . .
H51 H 0.2579 -0.1144 -0.1093 0.084 Uiso 1 1 calc R U . . .
C61 C 0.29118(14) 0.0745(5) -0.0715(2) 0.0555(11) Uani 1 1 d . U . . .
H61 H 0.2703 0.1334 -0.1085 0.067 Uiso 1 1 calc R U . . .
C12 C 0.29297(12) 0.4108(4) -0.0861(2) 0.0409(8) Uani 1 1 d . U . . .
C22 C 0.28807(14) 0.4104(6) -0.1578(2) 0.0655(13) Uani 1 1 d . U . . .
H22 H 0.3095 0.3669 -0.1677 0.079 Uiso 1 1 calc R U . . .
C32 C 0.25117(16) 0.4748(7) -0.2156(3) 0.0840(17) Uani 1 1 d . U . . .
H32 H 0.2479 0.4724 -0.2640 0.101 Uiso 1 1 calc R U . . .
C42 C 0.21953(15) 0.5416(6) -0.2023(3) 0.0726(14) Uani 1 1 d . U . . .
H42 H 0.1952 0.5862 -0.2411 0.087 Uiso 1 1 calc R U . . .
C52 C 0.22423(14) 0.5416(5) -0.1317(3) 0.0630(12) Uani 1 1 d . U . . .
H52 H 0.2026 0.5860 -0.1225 0.076 Uiso 1 1 calc R U . . .
C62 C 0.26034(12) 0.4772(5) -0.0731(2) 0.0496(10) Uani 1 1 d . U . . .
H62 H 0.2628 0.4782 -0.0252 0.059 Uiso 1 1 calc R U . . .
C13 C 0.34461(11) 0.3883(4) 0.07476(19) 0.0376(8) Uani 1 1 d . U . . .
C23 C 0.32289(13) 0.3162(5) 0.1095(2) 0.0479(10) Uani 1 1 d . U . . .
H23 H 0.3066 0.2327 0.0876 0.057 Uiso 1 1 calc R U . . .
C33 C 0.32516(14) 0.3667(5) 0.1755(2) 0.0587(11) Uani 1 1 d . U . . .
H33 H 0.3112 0.3163 0.1987 0.070 Uiso 1 1 calc R U . . .
C43 C 0.34855(14) 0.4933(6) 0.2071(2) 0.0630(12) Uani 1 1 d . U . . .
H43 H 0.3495 0.5301 0.2508 0.076 Uiso 1 1 calc R U . . .
C53 C 0.37021(15) 0.5639(5) 0.1739(2) 0.0622(12) Uani 1 1 d . U . . .
H53 H 0.3861 0.6483 0.1954 0.075 Uiso 1 1 calc R U . . .
C63 C 0.36878(13) 0.5117(5) 0.1091(2) 0.0489(10) Uani 1 1 d . U . . .
H63 H 0.3843 0.5599 0.0878 0.059 Uiso 1 1 calc R U . . .
C14 C 0.38168(15) 0.7020(5) -0.0937(3) 0.0600(12) Uani 1 1 d . U . . .
H14 H 0.3535 0.6698 -0.1275 0.072 Uiso 1 1 calc R U . . .
C24 C 0.39322(17) 0.8449(5) -0.0981(3) 0.0719(13) Uani 1 1 d . U . . .
H24 H 0.3732 0.9075 -0.1341 0.086 Uiso 1 1 calc R U . . .
C34 C 0.43489(17) 0.8921(6) -0.0479(3) 0.0790(14) Uani 1 1 d . U . . .
H34 H 0.4434 0.9877 -0.0492 0.095 Uiso 1 1 calc R U . . .
C44 C 0.46334(17) 0.7977(5) 0.0033(3) 0.0685(13) Uani 1 1 d . U . . .
H44 H 0.4917 0.8277 0.0373 0.082 Uiso 1 1 calc R U . . .
C54 C 0.44984(13) 0.6557(5) 0.0048(2) 0.0484(9) Uani 1 1 d . U . . .
C64 C 0.47908(14) 0.5524(5) 0.0597(2) 0.0539(11) Uani 1 1 d . U . . .
H64 H 0.5076 0.5798 0.0944 0.065 Uiso 1 1 calc R U . . .
C15 C 0.49264(13) 0.3190(5) 0.1123(2) 0.0458(9) Uani 1 1 d . U . . .
C25 C 0.53511(15) 0.3464(6) 0.1705(3) 0.0757(15) Uani 1 1 d . U . . .
H25 H 0.5468 0.4399 0.1781 0.091 Uiso 1 1 calc R U . . .
C35 C 0.55922(18) 0.2361(6) 0.2161(3) 0.0885(17) Uani 1 1 d . U . . .
H35 H 0.5877 0.2537 0.2540 0.106 Uiso 1 1 calc R U . . .
C45 C 0.54179(16) 0.1003(6) 0.2064(3) 0.0661(12) Uani 1 1 d . U . . .
C55 C 0.50022(15) 0.0678(6) 0.1501(3) 0.0686(13) Uani 1 1 d . U . . .
H55 H 0.4888 -0.0260 0.1437 0.082 Uiso 1 1 calc R U . . .
C65 C 0.47602(14) 0.1799(5) 0.1033(3) 0.0576(11) Uani 1 1 d . U . . .
H65 H 0.4478 0.1608 0.0648 0.069 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'
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'
Cu Cu 0.3201 1.2651 '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'
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
N1 Cu1 N2 79.09(13) . . ?
N1 Cu1 P1 117.01(9) . . ?
N2 Cu1 P1 124.54(9) . . ?
N1 Cu1 Br1 106.40(9) . . ?
N2 Cu1 Br1 108.15(9) . . ?
P1 Cu1 Br1 115.44(4) . . ?
C13 P1 C11 103.49(17) . . ?
C13 P1 C12 104.73(17) . . ?
C11 P1 C12 104.39(17) . . ?
C13 P1 Cu1 115.68(12) . . ?
C11 P1 Cu1 117.37(12) . . ?
C12 P1 Cu1 109.89(12) . . ?
C54 N1 C14 118.3(4) . . ?
C54 N1 Cu1 112.0(3) . . ?
C14 N1 Cu1 129.7(3) . . ?
C64 N2 C15 121.4(4) . . ?
C64 N2 Cu1 112.4(3) . . ?
C15 N2 Cu1 126.1(3) . . ?
O1 N3 O2 125.8(6) . . ?
O1 N3 C45 118.0(6) . . ?
O2 N3 C45 115.6(6) . . ?
C61 C11 C21 118.3(4) . . ?
C61 C11 P1 123.5(3) . . ?
C21 C11 P1 118.2(3) . . ?
C31 C21 C11 121.3(4) . . ?
C31 C21 H21 119.4 . . ?
C11 C21 H21 119.4 . . ?
C41 C31 C21 119.9(5) . . ?
C41 C31 H31 120.1 . . ?
C21 C31 H31 120.1 . . ?
C31 C41 C51 120.0(5) . . ?
C31 C41 H41 120.0 . . ?
C51 C41 H41 120.0 . . ?
C41 C51 C61 120.4(5) . . ?
C41 C51 H51 119.8 . . ?
C61 C51 H51 119.8 . . ?
C11 C61 C51 120.1(4) . . ?
C11 C61 H61 119.9 . . ?
C51 C61 H61 119.9 . . ?
C22 C12 C62 118.5(4) . . ?
C22 C12 P1 117.7(3) . . ?
C62 C12 P1 123.7(3) . . ?
C12 C22 C32 120.2(4) . . ?
C12 C22 H22 119.9 . . ?
C32 C22 H22 119.9 . . ?
C42 C32 C22 121.0(5) . . ?
C42 C32 H32 119.5 . . ?
C22 C32 H32 119.5 . . ?
C52 C42 C32 118.8(5) . . ?
C52 C42 H42 120.6 . . ?
C32 C42 H42 120.6 . . ?
C42 C52 C62 121.6(5) . . ?
C42 C52 H52 119.2 . . ?
C62 C52 H52 119.2 . . ?
C52 C62 C12 119.8(4) . . ?
C52 C62 H62 120.1 . . ?
C12 C62 H62 120.1 . . ?
C63 C13 C23 117.9(4) . . ?
C63 C13 P1 118.5(3) . . ?
C23 C13 P1 123.6(3) . . ?
C33 C23 C13 121.1(4) . . ?
C33 C23 H23 119.4 . . ?
C13 C23 H23 119.4 . . ?
C23 C33 C43 119.3(4) . . ?
C23 C33 H33 120.3 . . ?
C43 C33 H33 120.3 . . ?
C53 C43 C33 119.9(4) . . ?
C53 C43 H43 120.1 . . ?
C33 C43 H43 120.1 . . ?
C63 C53 C43 120.7(4) . . ?
C63 C53 H53 119.7 . . ?
C43 C53 H53 119.7 . . ?
C53 C63 C13 121.0(4) . . ?
C53 C63 H63 119.5 . . ?
C13 C63 H63 119.5 . . ?
N1 C14 C24 122.5(5) . . ?
N1 C14 H14 118.8 . . ?
C24 C14 H14 118.8 . . ?
C34 C24 C14 118.6(5) . . ?
C34 C24 H24 120.7 . . ?
C14 C24 H24 120.7 . . ?
C44 C34 C24 119.2(5) . . ?
C44 C34 H34 120.4 . . ?
C24 C34 H34 120.4 . . ?
C34 C44 C54 119.5(5) . . ?
C34 C44 H44 120.2 . . ?
C54 C44 H44 120.2 . . ?
N1 C54 C44 121.9(4) . . ?
N1 C54 C64 117.0(4) . . ?
C44 C54 C64 121.1(4) . . ?
N2 C64 C54 119.3(4) . . ?
N2 C64 H64 120.4 . . ?
C54 C64 H64 120.4 . . ?
C65 C15 C25 118.6(4) . . ?
C65 C15 N2 116.5(4) . . ?
C25 C15 N2 124.8(4) . . ?
C35 C25 C15 119.9(5) . . ?
C35 C25 H25 120.1 . . ?
C15 C25 H25 120.1 . . ?
C45 C35 C25 120.2(5) . . ?
C45 C35 H35 119.9 . . ?
C25 C35 H35 119.9 . . ?
C35 C45 C55 122.1(5) . . ?
C35 C45 N3 119.1(5) . . ?
C55 C45 N3 118.7(5) . . ?
C45 C55 C65 117.5(5) . . ?
C45 C55 H55 121.3 . . ?
C65 C55 H55 121.3 . . ?
C15 C65 C55 121.6(4) . . ?
C15 C65 H65 119.2 . . ?
C55 C65 H65 119.2 . . ?
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 N1 2.096(3) . ?
Cu1 N2 2.110(3) . ?
Cu1 P1 2.1952(10) . ?
Cu1 Br1 2.4212(7) . ?
P1 C13 1.822(4) . ?
P1 C11 1.824(4) . ?
P1 C12 1.831(4) . ?
N1 C54 1.332(5) . ?
N1 C14 1.334(5) . ?
N2 C64 1.275(5) . ?
N2 C15 1.411(5) . ?
N3 O1 1.181(6) . ?
N3 O2 1.256(6) . ?
N3 C45 1.488(7) . ?
C11 C61 1.383(5) . ?
C11 C21 1.387(5) . ?
C21 C31 1.379(6) . ?
C21 H21 0.9300 . ?
C31 C41 1.365(6) . ?
C31 H31 0.9300 . ?
C41 C51 1.374(6) . ?
C41 H41 0.9300 . ?
C51 C61 1.389(6) . ?
C51 H51 0.9300 . ?
C61 H61 0.9300 . ?
C12 C22 1.376(5) . ?
C12 C62 1.391(5) . ?
C22 C32 1.388(6) . ?
C22 H22 0.9300 . ?
C32 C42 1.366(6) . ?
C32 H32 0.9300 . ?
C42 C52 1.356(6) . ?
C42 H42 0.9300 . ?
C52 C62 1.382(6) . ?
C52 H52 0.9300 . ?
C62 H62 0.9300 . ?
C13 C63 1.384(5) . ?
C13 C23 1.396(5) . ?
C23 C33 1.378(5) . ?
C23 H23 0.9300 . ?
C33 C43 1.387(6) . ?
C33 H33 0.9300 . ?
C43 C53 1.366(6) . ?
C43 H43 0.9300 . ?
C53 C63 1.371(6) . ?
C53 H53 0.9300 . ?
C63 H63 0.9300 . ?
C14 C24 1.385(6) . ?
C14 H14 0.9300 . ?
C24 C34 1.375(7) . ?
C24 H24 0.9300 . ?
C34 C44 1.354(6) . ?
C34 H34 0.9300 . ?
C44 C54 1.389(6) . ?
C44 H44 0.9300 . ?
C54 C64 1.448(6) . ?
C64 H64 0.9300 . ?
C15 C65 1.376(6) . ?
C15 C25 1.400(5) . ?
C25 C35 1.359(7) . ?
C25 H25 0.9300 . ?
C35 C45 1.357(7) . ?
C35 H35 0.9300 . ?
C45 C55 1.375(6) . ?
C55 C65 1.382(6) . ?
C55 H55 0.9300 . ?
C65 H65 0.9300 . ?
