#------------------------------------------------------------------------------
#$Date: 2023-01-04 04:13:08 +0200 (Wed, 04 Jan 2023) $
#$Revision: 280092 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/60/7246075.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_7246075
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         'C32 H30 Br Cu N3 P'
_chemical_formula_sum            'C32 H30 Br Cu N3 P'
_chemical_formula_weight         631.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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                 97.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.36873(18)
_cell_length_b                   12.5828(3)
_cell_length_c                   25.2196(6)
_cell_measurement_reflns_used    4776
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.664
_cell_measurement_theta_min      3.880
_cell_volume                     2947.00(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25850
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         3.851
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Oxford Diffraction, 2009)'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       fragments
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.70
_exptl_transmission_factor_min   0.58
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5779
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0320
_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)+(0.0396P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4150
_reflns_number_total             5779
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra05341a2.cif
_cod_data_source_block           6
_cod_original_cell_volume        2947.00(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7246075
_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+1/2, -z+1/2'
'-x, -y, -z'
'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 0.37415(3) 0.10738(2) 0.39052(2) 0.04178(10) Uani 1 1 d . U . . .
Br1 Br 0.22007(3) -0.04349(2) 0.37753(2) 0.05164(10) Uani 1 1 d . U . . .
P1 P 0.36136(6) 0.24762(5) 0.33868(2) 0.03792(15) Uani 1 1 d . U . . .
N1 N 0.59425(19) 0.06836(15) 0.40290(8) 0.0410(5) Uani 1 1 d . U . . .
N2 N 0.42473(18) 0.14754(15) 0.47171(7) 0.0367(4) Uani 1 1 d . U . . .
N3 N 0.0204(3) 0.3123(2) 0.59626(11) 0.0825(8) Uani 1 1 d . U . . .
C11 C 0.4698(3) 0.3525(2) 0.37364(9) 0.0435(5) Uani 1 1 d . U . . .
C21 C 0.6184(3) 0.3446(2) 0.37984(11) 0.0581(7) Uani 1 1 d . U . . .
H21 H 0.6618 0.2900 0.3629 0.070 Uiso 1 1 calc R U . . .
C31 C 0.7036(4) 0.4178(3) 0.41123(13) 0.0775(9) Uani 1 1 d . U . . .
H31 H 0.8034 0.4128 0.4149 0.093 Uiso 1 1 calc R U . . .
C41 C 0.6389(4) 0.4972(3) 0.43663(13) 0.0794(9) Uani 1 1 d . U . . .
H41 H 0.6953 0.5465 0.4574 0.095 Uiso 1 1 calc R U . . .
C51 C 0.4933(4) 0.5047(3) 0.43182(12) 0.0748(8) Uani 1 1 d . U . . .
H51 H 0.4507 0.5584 0.4496 0.090 Uiso 1 1 calc R U . . .
C61 C 0.4086(3) 0.4330(2) 0.40076(10) 0.0581(7) Uani 1 1 d . U . . .
H61 H 0.3089 0.4386 0.3979 0.070 Uiso 1 1 calc R U . . .
C12 C 0.4396(2) 0.22826(19) 0.27660(9) 0.0383(5) Uani 1 1 d . U . . .
C22 C 0.5112(3) 0.3055(2) 0.25186(10) 0.0586(7) Uani 1 1 d . U . . .
H22 H 0.5228 0.3729 0.2670 0.070 Uiso 1 1 calc R U . . .
C32 C 0.5662(3) 0.2838(3) 0.20469(11) 0.0687(8) Uani 1 1 d . U . . .
H32 H 0.6147 0.3365 0.1883 0.082 Uiso 1 1 calc R U . . .
C42 C 0.5495(3) 0.1870(3) 0.18255(11) 0.0656(7) Uani 1 1 d . U . . .
H42 H 0.5891 0.1724 0.1514 0.079 Uiso 1 1 calc R U . . .
C52 C 0.4756(3) 0.1102(3) 0.20493(11) 0.0688(8) Uani 1 1 d . U . . .
H52 H 0.4610 0.0444 0.1883 0.083 Uiso 1 1 calc R U . . .
C62 C 0.4221(3) 0.1296(2) 0.25261(10) 0.0547(7) Uani 1 1 d . U . . .
H62 H 0.3742 0.0761 0.2685 0.066 Uiso 1 1 calc R U . . .
C13 C 0.1890(2) 0.3091(2) 0.31389(9) 0.0449(6) Uani 1 1 d . U . . .
C23 C 0.1755(3) 0.4062(2) 0.28812(11) 0.0639(7) Uani 1 1 d . U . . .
H23 H 0.2573 0.4464 0.2852 0.077 Uiso 1 1 calc R U . . .
C33 C 0.0422(4) 0.4444(3) 0.26659(13) 0.0798(9) Uani 1 1 d . U . . .
H33 H 0.0343 0.5094 0.2489 0.096 Uiso 1 1 calc R U . . .
C43 C -0.0776(4) 0.3858(3) 0.27153(14) 0.0890(10) Uani 1 1 d . U . . .
H43 H -0.1676 0.4125 0.2579 0.107 Uiso 1 1 calc R U . . .
C53 C -0.0683(3) 0.2890(3) 0.29597(14) 0.0868(10) Uani 1 1 d . U . . .
H53 H -0.1508 0.2488 0.2979 0.104 Uiso 1 1 calc R U . . .
C63 C 0.0663(3) 0.2510(3) 0.31806(11) 0.0630(8) Uani 1 1 d . U . . .
H63 H 0.0733 0.1859 0.3357 0.076 Uiso 1 1 calc R U . . .
C14 C 0.6824(3) 0.0359(2) 0.36826(11) 0.0530(7) Uani 1 1 d . U . . .
H14 H 0.6428 0.0196 0.3335 0.064 Uiso 1 1 calc R U . . .
C24 C 0.8281(3) 0.0259(2) 0.38196(12) 0.0579(7) Uani 1 1 d . U . . .
H24 H 0.8856 0.0039 0.3566 0.069 Uiso 1 1 calc R U . . .
C34 C 0.8882(3) 0.0482(2) 0.43273(12) 0.0622(7) Uani 1 1 d . U . . .
H34 H 0.9870 0.0418 0.4426 0.075 Uiso 1 1 calc R U . . .
C44 C 0.8006(3) 0.0803(2) 0.46926(11) 0.0578(7) Uani 1 1 d . U . . .
H44 H 0.8390 0.0948 0.5044 0.069 Uiso 1 1 calc R U . . .
C54 C 0.6541(2) 0.0909(2) 0.45305(10) 0.0418(5) Uani 1 1 d . U . . .
C64 C 0.5573(2) 0.1307(2) 0.48932(10) 0.0435(6) Uani 1 1 d . U . . .
H64 H 0.5917 0.1437 0.5250 0.052 Uiso 1 1 calc R U . . .
C15 C 0.3276(2) 0.18910(18) 0.50523(9) 0.0382(5) Uani 1 1 d . U . . .
C25 C 0.3536(3) 0.1935(2) 0.56036(9) 0.0456(6) Uani 1 1 d . U . . .
H25 H 0.4414 0.1696 0.5779 0.055 Uiso 1 1 calc R U . . .
C35 C 0.2526(3) 0.2325(2) 0.58958(11) 0.0557(7) Uani 1 1 d . U . . .
H35 H 0.2726 0.2329 0.6267 0.067 Uiso 1 1 calc R U . . .
C45 C 0.1200(3) 0.2718(2) 0.56553(11) 0.0535(6) Uani 1 1 d . U . . .
C55 C 0.0955(3) 0.2676(2) 0.51035(11) 0.0599(7) Uani 1 1 d . U . . .
H55 H 0.0090 0.2932 0.4927 0.072 Uiso 1 1 calc R U . . .
C65 C 0.1959(2) 0.2264(2) 0.48090(10) 0.0521(7) Uani 1 1 d . U . . .
H65 H 0.1750 0.2235 0.4438 0.063 Uiso 1 1 calc R U . . .
C75 C 0.0396(4) 0.3017(4) 0.65361(14) 0.1081(13) Uani 1 1 d . U . . .
H75A H 0.0594 0.2288 0.6631 0.162 Uiso 1 1 calc R U . . .
H75B H -0.0466 0.3240 0.6672 0.162 Uiso 1 1 calc R U . . .
H75C H 0.1187 0.3454 0.6687 0.162 Uiso 1 1 calc R U . . .
C85 C -0.1154(4) 0.3504(4) 0.57179(16) 0.1128(14) Uani 1 1 d . U . . .
H85A H -0.1010 0.4064 0.5472 0.169 Uiso 1 1 calc R U . . .
H85B H -0.1692 0.3771 0.5988 0.169 Uiso 1 1 calc R U . . .
H85C H -0.1678 0.2934 0.5528 0.169 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'
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 79.68(7) . . ?
N1 Cu1 P1 104.60(5) . . ?
N2 Cu1 P1 112.05(6) . . ?
N1 Cu1 Br1 113.52(6) . . ?
N2 Cu1 Br1 112.36(5) . . ?
P1 Cu1 Br1 125.16(2) . . ?
C11 P1 C13 105.70(12) . . ?
C11 P1 C12 104.46(11) . . ?
C13 P1 C12 101.51(10) . . ?
C11 P1 Cu1 108.17(8) . . ?
C13 P1 Cu1 121.50(9) . . ?
C12 P1 Cu1 114.00(8) . . ?
C54 N1 C14 117.4(2) . . ?
C54 N1 Cu1 111.71(15) . . ?
C14 N1 Cu1 130.54(17) . . ?
C64 N2 C15 121.53(19) . . ?
C64 N2 Cu1 112.43(15) . . ?
C15 N2 Cu1 126.04(14) . . ?
C45 N3 C85 120.7(3) . . ?
C45 N3 C75 121.6(3) . . ?
C85 N3 C75 116.9(3) . . ?
C21 C11 C61 118.1(2) . . ?
C21 C11 P1 119.5(2) . . ?
C61 C11 P1 121.8(2) . . ?
C11 C21 C31 120.6(3) . . ?
C11 C21 H21 119.7 . . ?
C31 C21 H21 119.7 . . ?
C41 C31 C21 119.4(3) . . ?
C41 C31 H31 120.3 . . ?
C21 C31 H31 120.3 . . ?
C51 C41 C31 120.7(3) . . ?
C51 C41 H41 119.7 . . ?
C31 C41 H41 119.7 . . ?
C41 C51 C61 120.2(3) . . ?
C41 C51 H51 119.9 . . ?
C61 C51 H51 119.9 . . ?
C51 C61 C11 120.9(3) . . ?
C51 C61 H61 119.5 . . ?
C11 C61 H61 119.5 . . ?
C22 C12 C62 118.2(2) . . ?
C22 C12 P1 124.6(2) . . ?
C62 C12 P1 117.17(18) . . ?
C12 C22 C32 120.6(3) . . ?
C12 C22 H22 119.7 . . ?
C32 C22 H22 119.7 . . ?
C42 C32 C22 120.0(3) . . ?
C42 C32 H32 120.0 . . ?
C22 C32 H32 120.0 . . ?
C32 C42 C52 120.9(3) . . ?
C32 C42 H42 119.6 . . ?
C52 C42 H42 119.6 . . ?
C42 C52 C62 119.9(3) . . ?
C42 C52 H52 120.0 . . ?
C62 C52 H52 120.0 . . ?
C12 C62 C52 120.3(3) . . ?
C12 C62 H62 119.9 . . ?
C52 C62 H62 119.9 . . ?
C63 C13 C23 118.7(2) . . ?
C63 C13 P1 117.2(2) . . ?
C23 C13 P1 124.0(2) . . ?
C13 C23 C33 121.0(3) . . ?
C13 C23 H23 119.5 . . ?
C33 C23 H23 119.5 . . ?
C43 C33 C23 119.3(3) . . ?
C43 C33 H33 120.3 . . ?
C23 C33 H33 120.3 . . ?
C53 C43 C33 121.4(3) . . ?
C53 C43 H43 119.3 . . ?
C33 C43 H43 119.3 . . ?
C43 C53 C63 119.2(3) . . ?
C43 C53 H53 120.4 . . ?
C63 C53 H53 120.4 . . ?
C13 C63 C53 120.4(3) . . ?
C13 C63 H63 119.8 . . ?
C53 C63 H63 119.8 . . ?
N1 C14 C24 122.9(3) . . ?
N1 C14 H14 118.6 . . ?
C24 C14 H14 118.6 . . ?
C34 C24 C14 119.6(3) . . ?
C34 C24 H24 120.2 . . ?
C14 C24 H24 120.2 . . ?
C24 C34 C44 118.9(2) . . ?
C24 C34 H34 120.6 . . ?
C44 C34 H34 120.6 . . ?
C34 C44 C54 119.1(3) . . ?
C34 C44 H44 120.4 . . ?
C54 C44 H44 120.4 . . ?
N1 C54 C44 122.1(2) . . ?
N1 C54 C64 116.4(2) . . ?
C44 C54 C64 121.4(2) . . ?
N2 C64 C54 119.6(2) . . ?
N2 C64 H64 120.2 . . ?
C54 C64 H64 120.2 . . ?
C25 C15 C65 117.5(2) . . ?
C25 C15 N2 124.9(2) . . ?
C65 C15 N2 117.6(2) . . ?
C35 C25 C15 121.0(2) . . ?
C35 C25 H25 119.5 . . ?
C15 C25 H25 119.5 . . ?
C25 C35 C45 122.2(3) . . ?
C25 C35 H35 118.9 . . ?
C45 C35 H35 118.9 . . ?
N3 C45 C55 122.9(3) . . ?
N3 C45 C35 120.8(3) . . ?
C55 C45 C35 116.3(2) . . ?
C65 C55 C45 121.7(2) . . ?
C65 C55 H55 119.2 . . ?
C45 C55 H55 119.2 . . ?
C55 C65 C15 121.4(2) . . ?
C55 C65 H65 119.3 . . ?
C15 C65 H65 119.3 . . ?
N3 C75 H75A 109.5 . . ?
N3 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
N3 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N3 C85 H85A 109.5 . . ?
N3 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
N3 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
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 2.1026(18) . ?
Cu1 N2 2.1015(18) . ?
Cu1 P1 2.1900(7) . ?
Cu1 Br1 2.3812(4) . ?
P1 C11 1.820(2) . ?
P1 C13 1.825(2) . ?
P1 C12 1.831(2) . ?
N1 C54 1.344(3) . ?
N1 C14 1.342(3) . ?
N2 C64 1.281(3) . ?
N2 C15 1.421(3) . ?
N3 C45 1.386(3) . ?
N3 C85 1.423(4) . ?
N3 C75 1.440(4) . ?
C11 C21 1.383(3) . ?
C11 C61 1.389(4) . ?
C21 C31 1.395(4) . ?
C21 H21 0.9300 . ?
C31 C41 1.371(5) . ?
C31 H31 0.9300 . ?
C41 C51 1.356(4) . ?
C41 H41 0.9300 . ?
C51 C61 1.376(4) . ?
C51 H51 0.9300 . ?
C61 H61 0.9300 . ?
C12 C22 1.377(3) . ?
C12 C62 1.381(3) . ?
C22 C32 1.384(4) . ?
C22 H22 0.9300 . ?
C32 C42 1.341(4) . ?
C32 H32 0.9300 . ?
C42 C52 1.355(4) . ?
C42 H42 0.9300 . ?
C52 C62 1.384(4) . ?
C52 H52 0.9300 . ?
C62 H62 0.9300 . ?
C13 C63 1.379(4) . ?
C13 C23 1.381(4) . ?
C23 C33 1.380(4) . ?
C23 H23 0.9300 . ?
C33 C43 1.362(5) . ?
C33 H33 0.9300 . ?
C43 C53 1.363(5) . ?
C43 H43 0.9300 . ?
C53 C63 1.395(4) . ?
C53 H53 0.9300 . ?
C63 H63 0.9300 . ?
C14 C24 1.369(3) . ?
C14 H14 0.9300 . ?
C24 C34 1.358(4) . ?
C24 H24 0.9300 . ?
C34 C44 1.373(4) . ?
C34 H34 0.9300 . ?
C44 C54 1.385(3) . ?
C44 H44 0.9300 . ?
C54 C64 1.459(3) . ?
C64 H64 0.9300 . ?
C15 C25 1.381(3) . ?
C15 C65 1.385(3) . ?
C25 C35 1.365(3) . ?
C25 H25 0.9300 . ?
C35 C45 1.399(4) . ?
C35 H35 0.9300 . ?
C45 C55 1.381(4) . ?
C55 C65 1.374(3) . ?
C55 H55 0.9300 . ?
C65 H65 0.9300 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
C85 H85A 0.9600 . ?
C85 H85B 0.9600 . ?
C85 H85C 0.9600 . ?
