#------------------------------------------------------------------------------
#$Date: 2024-04-05 07:51:22 +0200 (Fri 05 de Apr de 2024) $
#$Revision: 291083 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/13/1571382.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_1571382
loop_
_publ_author_name
'Yamba, Zaina'
'Peoble, Anna'
'Novikov, Egor'
'Castañeda, Raúl'
'Timofeeva, Tatiana'
_publ_section_title
;
 Interplay of Isomorphs and Polymorphs of Amidino-Copper(II) Complexes
 with Different Halides
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              319
_journal_paper_doi               10.3390/cryst14040319
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C5 H6 Br2 Cu N4'
_chemical_formula_sum            'C5 H6 Br2 Cu N4'
_chemical_formula_weight         345.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-02-27
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9430(2)
_cell_length_b                   6.4316(2)
_cell_length_c                   15.2113(3)
_cell_measurement_reflns_used    2781
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8810
_cell_measurement_theta_min      5.7130
_cell_volume                     874.92(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.71a 64-bit (release 17-04-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.71a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     36.00 107.00   0.50    2.00    --  105.25-109.00 -41.00  142
  2  ω     33.00  75.00   0.50    2.00    --  105.25 -61.00   0.00   84
  3  ω     24.00 118.00   0.50    0.50    --   46.66  77.00-120.00  188
  4  ω    -41.00  26.00   0.50    0.50    --  -46.66  38.00-162.00  134
  5  ω    -30.00  29.00   0.50    0.50    --  -46.66  19.00-150.00  118
  6  ω    -30.00  29.00   0.50    0.50    --  -46.66  19.00 -30.00  118
  7  ω    -30.00  29.00   0.50    0.50    --  -46.66  19.00  60.00  118
  8  ω    -65.00 -30.00   0.50    2.00    -- -103.00  61.00 -30.00   70
  9  ω    -65.00 -30.00   0.50    2.00    -- -103.00  61.00   0.00   70
 10  ω    -65.00 -30.00   0.50    2.00    -- -103.00  61.00  60.00   70
 11  ω   -118.00 -47.00   0.50    0.50    --  -46.66 -77.00  90.00  142
 12  ω   -174.00 -90.00   0.50    2.00    -- -103.00 -38.00  42.00  168
 13  ω   -173.00 -82.00   0.50    2.00    -- -103.00-109.00 -41.00  182
 14  ω   -174.00 -79.00   0.50    2.00    -- -103.00 -88.00-148.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4491
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.970
_diffrn_reflns_theta_min         5.739
_exptl_absorpt_coefficient_mu    13.814
_exptl_absorpt_correction_T_max  0.75361
_exptl_absorpt_correction_T_min  0.73960
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.71a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.623
_exptl_crystal_description       sphere
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.014
_refine_diff_density_max         3.220
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         903
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0562
_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)+(0.1255P)²+0.7473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                839
_reflns_number_total             903
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Crystals-CIFS.cif
_cod_data_source_block           7
_cod_database_code               1571382
_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   0.874
_shelx_estimated_absorpt_t_min   0.545
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-H2 = N3-H3A = N3-H3B
 0.9 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Br2 Br 0.38532(9) 0.250000 0.53644(5) 0.0217(4) Uani 1 2 d S T P . .
Br1 Br 0.47224(9) 0.250000 0.31305(5) 0.0250(4) Uani 1 2 d S T P . .
Cu1 Cu 0.60755(12) 0.250000 0.44929(8) 0.0208(4) Uani 1 2 d S T P . .
N3 N 1.0631(7) 0.250000 0.4074(5) 0.0199(13) Uani 1 2 d DS T P . .
H3A H 1.080(10) 0.250000 0.3492(17) 0.010(19) Uiso 1 2 d DS . P . .
H3B H 1.152(9) 0.250000 0.435(10) 0.08(5) Uiso 1 2 d DS . P . .
N1 N 0.7495(8) 0.250000 0.5568(4) 0.0175(13) Uani 1 2 d S T P . .
N4 N 0.9719(7) 0.250000 0.6848(4) 0.0229(16) Uani 1 2 d S T P . .
N2 N 0.8015(8) 0.250000 0.3907(5) 0.0228(15) Uani 1 2 d DS T P . .
H2 H 0.826(16) 0.250000 0.333(3) 0.06(4) Uiso 1 2 d DS . P . .
C6 C 0.9184(9) 0.250000 0.4376(5) 0.0192(16) Uani 1 2 d S T P . .
C5 C 0.8950(9) 0.250000 0.5349(5) 0.0206(18) Uani 1 2 d S T P . .
C4 C 1.0038(9) 0.250000 0.5981(5) 0.0196(16) Uani 1 2 d S T P . .
H4 H 1.105612 0.250000 0.580228 0.024 Uiso 1 2 calc R U P . .
C1 C 0.7151(8) 0.250000 0.6426(5) 0.0207(16) Uani 1 2 d S T P . .
H1 H 0.613131 0.250000 0.660052 0.025 Uiso 1 2 calc R U P . .
C2 C 0.8248(10) 0.250000 0.7055(5) 0.0275(18) Uani 1 2 d S T P . .
H2A H 0.796539 0.250000 0.765696 0.033 Uiso 1 2 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 -2 0.0010
1 0 2 0.0137
0 2 1 0.0200
0 -2 -1 0.0239
0 0 1 0.0114
0 0 -1 0.0010
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
Br2 Cu1 Br1 93.43(5) . . ?
N1 Cu1 Br2 94.13(19) . . ?
N1 Cu1 Br1 172.4(2) . . ?
N2 Cu1 Br2 173.5(2) . . ?
N2 Cu1 Br1 93.1(2) . . ?
N2 Cu1 N1 79.4(3) . . ?
H3A N3 H3B 108(10) . . ?
C6 N3 H3A 119(6) . . ?
C6 N3 H3B 132(10) . . ?
C5 N1 Cu1 113.5(5) . . ?
C1 N1 Cu1 128.9(6) . . ?
C1 N1 C5 117.6(7) . . ?
C4 N4 C2 115.7(7) . . ?
Cu1 N2 H2 131(10) . . ?
C6 N2 Cu1 118.5(6) . . ?
C6 N2 H2 110(10) . . ?
N3 C6 C5 117.6(7) . . ?
N2 C6 N3 126.1(8) . . ?
N2 C6 C5 116.3(7) . . ?
N1 C5 C6 112.4(7) . . ?
N1 C5 C4 121.0(7) . . ?
C4 C5 C6 126.6(7) . . ?
N4 C4 C5 122.4(7) . . ?
N4 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
N1 C1 H1 119.5 . . ?
N1 C1 C2 121.0(7) . . ?
C2 C1 H1 119.5 . . ?
N4 C2 C1 122.2(7) . . ?
N4 C2 H2A 118.9 . . ?
C1 C2 H2A 118.9 . . ?
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
Br2 Cu1 2.3889(14) . ?
Br1 Cu1 2.3997(13) . ?
Cu1 N1 2.070(7) . ?
Cu1 N2 1.950(7) . ?
N3 H3A 0.90(2) . ?
N3 H3B 0.90(2) . ?
N3 C6 1.373(11) . ?
N1 C5 1.343(11) . ?
N1 C1 1.341(10) . ?
N4 C4 1.350(9) . ?
N4 C2 1.353(12) . ?
N2 H2 0.90(2) . ?
N2 C6 1.266(11) . ?
C6 C5 1.495(11) . ?
C5 C4 1.367(12) . ?
C4 H4 0.9500 . ?
C1 H1 0.9500 . ?
C1 C2 1.370(12) . ?
C2 H2A 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
Cu1 N1 C5 C6 0.000(2) . . . . ?
Cu1 N1 C5 C4 180.000(2) . . . . ?
Cu1 N1 C1 C2 180.000(2) . . . . ?
Cu1 N2 C6 N3 180.000(1) . . . . ?
Cu1 N2 C6 C5 0.000(2) . . . . ?
N3 C6 C5 N1 180.000(2) . . . . ?
N3 C6 C5 C4 0.000(2) . . . . ?
N1 C5 C4 N4 0.000(3) . . . . ?
N1 C1 C2 N4 0.000(3) . . . . ?
N2 C6 C5 N1 0.000(2) . . . . ?
N2 C6 C5 C4 180.000(2) . . . . ?
C6 C5 C4 N4 180.000(2) . . . . ?
C5 N1 C1 C2 0.000(3) . . . . ?
C4 N4 C2 C1 0.000(3) . . . . ?
C1 N1 C5 C6 180.000(2) . . . . ?
C1 N1 C5 C4 0.000(3) . . . . ?
C2 N4 C4 C5 0.000(3) . . . . ?
