#------------------------------------------------------------------------------
#$Date: 2019-10-30 06:27:02 +0200 (Wed, 30 Oct 2019) $
#$Revision: 220529 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/89/7058954.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_7058954
loop_
_publ_author_name
'Berezin, Alexey Sergeevich'
'Komarovskikh, Andrey'
'Syrokvashin, Mikhail M.'
'Sheven, Dmitry G.'
'Komarov, Vladislav'
_publ_section_title
;
 Trinuclear Copper(II) Bromide Complex [C3H5N3Br]2n[Cu3Br8]n. Structure,
 Magnetic Properties and DFT calculations.
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C9NJ04826J
_journal_year                    2019
_chemical_formula_moiety         'Br8 Cu3, 2(C3 H5 Br N3)'
_chemical_formula_sum            'C6 H10 Br10 Cu3 N6'
_chemical_formula_weight         1155.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.    2019-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                67.660(3)
_cell_angle_beta                 89.706(4)
_cell_angle_gamma                86.172(4)
_cell_formula_units_Z            1
_cell_length_a                   3.9511(3)
_cell_length_b                   12.1653(10)
_cell_length_c                   12.6022(10)
_cell_measurement_reflns_used    2261
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.96
_cell_volume                     558.89(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6106
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.640
_diffrn_reflns_theta_min         1.814
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    20.708
_exptl_absorpt_correction_T_max  0.4322
_exptl_absorpt_correction_T_min  0.1797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1396 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.4158. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    3.434
_exptl_crystal_description       prism
_exptl_crystal_F_000             525
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.107
_refine_diff_density_max         1.102
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         3146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0394
_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)+(0.0471P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2523
_reflns_number_total             3146
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj04826j10.cif
_cod_data_source_block           cuoaecphbr
_cod_database_code               7058954
_shelx_shelxl_version_number     2014/7
_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   0.215
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C3(H3)
2.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Br3A Br 0.37288(12) 1.05116(5) 0.62162(4) 0.00983(12) Uani 1 1 d . . .
Br4A Br 0.05819(13) 0.79770(5) 0.64162(4) 0.01133(13) Uani 1 1 d . . .
Br2A Br 0.43843(13) 0.65009(5) 0.90876(4) 0.01211(13) Uani 1 1 d . . .
Br1A Br 0.78600(13) 0.91683(5) 0.88293(4) 0.01293(13) Uani 1 1 d . . .
Br1C Br 0.80719(15) 0.34059(6) 0.57030(5) 0.01910(15) Uani 1 1 d . . .
Cu2 Cu 0.0000 1.0000 0.5000 0.0116(2) Uani 1 2 d S T P
Cu1 Cu 0.38945(16) 0.85317(6) 0.77786(5) 0.01145(15) Uani 1 1 d . . .
N2 N 1.0940(12) 0.3641(5) 0.8645(4) 0.0203(11) Uani 1 1 d . . .
H2 H 1.1942 0.3369 0.9327 0.024 Uiso 1 1 calc R . .
N1 N 0.9316(13) 0.4742(5) 0.8126(4) 0.0238(12) Uani 1 1 d . . .
H1 H 0.9071 0.5292 0.8420 0.029 Uiso 1 1 calc R . .
C2 C 0.9027(13) 0.3812(5) 0.6955(4) 0.0123(11) Uani 1 1 d . . .
C1 C 1.0772(13) 0.3035(5) 0.7954(4) 0.0131(11) Uani 1 1 d . . .
N3 N 1.2228(13) 0.1939(5) 0.8199(4) 0.0237(12) Uani 1 1 d . . .
H3A H 1.3383 0.1572 0.8848 0.028 Uiso 1 1 calc R . .
H3B H 1.2032 0.1585 0.7712 0.028 Uiso 1 1 calc R . .
C3 C 0.8169(15) 0.4845(6) 0.7106(5) 0.0201(13) Uani 1 1 d . . .
H3 H 0.6949 0.5527 0.6567 0.024 Uiso 1 1 calc R . .
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
Cu2 Br3A Cu1 94.45(2) . .
Cu2 Br4A Cu1 93.49(2) . .
Br3A Cu2 Br3A 180.0 . 2_576
Br3A Cu2 Br4A 93.082(18) 2_576 .
Br3A Cu2 Br4A 86.917(18) . .
Br3A Cu2 Br4A 86.919(18) 2_576 2_576
Br3A Cu2 Br4A 93.082(19) . 2_576
Br4A Cu2 Br4A 180.0 2_576 .
Br3A Cu1 Br4A 84.54(3) . .
Br2A Cu1 Br3A 171.46(3) . .
Br2A Cu1 Br4A 90.34(3) . .
Br2A Cu1 Br1A 94.17(3) . .
Br1A Cu1 Br3A 89.80(3) . .
Br1A Cu1 Br4A 169.54(3) . .
N1 N2 H2 125.3 . .
C1 N2 H2 125.3 . .
C1 N2 N1 109.4(5) . .
N2 N1 H1 125.7 . .
C3 N1 N2 108.6(5) . .
C3 N1 H1 125.7 . .
C1 C2 Br1C 123.7(4) . .
C3 C2 Br1C 128.9(4) . .
C3 C2 C1 107.4(5) . .
N2 C1 C2 106.0(5) . .
N3 C1 N2 124.0(5) . .
N3 C1 C2 129.8(5) . .
C1 N3 H3A 120.0 . .
C1 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
N1 C3 C2 108.7(5) . .
N1 C3 H3 125.7 . .
C2 C3 H3 125.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br3A Cu2 2.4037(5) .
Br3A Cu1 2.4613(8) .
Br4A Cu2 2.4258(5) .
Br4A Cu1 2.4775(8) .
Br2A Cu1 2.3882(8) .
Br1A Cu1 2.4022(8) .
Br1C C2 1.871(5) .
Cu2 Br3A 2.4037(5) 2_576
Cu2 Br4A 2.4258(5) 2_576
N2 H2 0.8800 .
N2 N1 1.363(7) .
N2 C1 1.341(7) .
N1 H1 0.8800 .
N1 C3 1.323(7) .
C2 C1 1.404(7) .
C2 C3 1.361(8) .
C1 N3 1.338(7) .
N3 H3A 0.8800 .
N3 H3B 0.8800 .
C3 H3 0.9500 .
