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#$Date: 2023-05-11 01:44:56 +0300 (Thu, 11 May 2023) $
#$Revision: 283661 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712997.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_7712997
loop_
_publ_author_name
'Belikova, Daria E.'
'Fateev, Sergey A.'
'Khrustalev, Victor N.'
'Marchenko, Ekaterina I.'
'Goodilin, Eugene A.'
'Wang, Shenghao'
'Tarasov, Alexey B.'
_publ_section_title
;
 Exceptional structural diversity of hybrid halocuprates(I) with
 methylammonium and formamidinium cations.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00687e
_journal_year                    2023
_chemical_formula_moiety         'Br4 Cu3, C6 H15 N2 O2'
_chemical_formula_sum            'C6 H15 Br4 Cu3 N2 O2'
_chemical_formula_weight         657.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7900(9)
_cell_length_b                   15.8919(8)
_cell_length_c                   6.2660(3)
_cell_measurement_reflns_used    3996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.70
_cell_measurement_theta_min      2.56
_cell_volume                     1572.35(14)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2018)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'SHELXTL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-III CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            29951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.586
_diffrn_reflns_theta_min         2.563
_exptl_absorpt_coefficient_mu    14.176
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.777
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00039(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0332
_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)+(0.0241P)²+2.46P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1705
_reflns_number_total             2860
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00687e2.cif
_cod_data_source_block           HDMF2Cu3Br4
_cod_database_code               7712997
_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   0.139
_shelx_estimated_absorpt_t_max   0.765
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, 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
Br1 Br 0.33274(2) 0.15872(2) 0.35836(6) 0.01411(8) Uani 1 1 d . . . . .
Br2 Br 0.50318(2) 0.33790(2) 0.35487(6) 0.01781(9) Uani 1 1 d . . . . .
Cu1 Cu 0.2500 0.2500 0.10834(11) 0.02159(15) Uani 1 2 d S T P . .
Cu2 Cu 0.43024(3) 0.24783(3) 0.10973(9) 0.02604(13) Uani 1 1 d . . . . .
O1 O 0.73031(18) 0.32351(17) 0.5916(4) 0.0216(6) Uani 1 1 d . . . . .
H1O H 0.7500 0.2500 0.610(10) 0.032 Uiso 1 2 d S U P . .
N1 N 0.6411(2) 0.4230(2) 0.7146(5) 0.0166(7) Uani 1 1 d . . . . .
C1 C 0.6687(3) 0.3456(2) 0.7101(6) 0.0160(7) Uani 1 1 d . . . . .
H1 H 0.6420 0.3046 0.7977 0.019 Uiso 1 1 calc R U . . .
C2 C 0.6761(3) 0.4875(3) 0.5730(8) 0.0283(10) Uani 1 1 d . . . . .
H2A H 0.6712 0.5428 0.6412 0.042 Uiso 1 1 calc R U . . .
H2B H 0.6447 0.4877 0.4381 0.042 Uiso 1 1 calc R U . . .
H2C H 0.7359 0.4752 0.5448 0.042 Uiso 1 1 calc R U . . .
C3 C 0.5683(3) 0.4457(2) 0.8461(6) 0.0205(8) Uani 1 1 d . . . . .
H3A H 0.5834 0.4931 0.9387 0.031 Uiso 1 1 calc R U . . .
H3B H 0.5518 0.3975 0.9340 0.031 Uiso 1 1 calc R U . . .
H3C H 0.5209 0.4619 0.7538 0.031 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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3DT00687E 2023
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
Cu1 Br1 Cu1 77.488(11) 7_566 . ?
Cu1 Br1 Cu2 111.542(19) 7_566 . ?
Cu1 Br1 Cu2 67.638(16) . . ?
Cu1 Br1 Cu2 66.885(16) 7_566 7_566 ?
Cu1 Br1 Cu2 110.463(18) . 7_566 ?
Cu2 Br1 Cu2 73.055(14) . 7_566 ?
Cu2 Br2 Cu2 81.737(16) 7_566 . ?
Br1 Cu1 Br1 102.52(3) 8_655 7_565 ?
Br1 Cu1 Br1 117.073(16) 8_655 2 ?
Br1 Cu1 Br1 109.163(14) 7_565 2 ?
Br1 Cu1 Br1 109.162(14) 8_655 . ?
Br1 Cu1 Br1 117.073(16) 7_565 . ?
Br1 Cu1 Br1 102.51(3) 2 . ?
Br2 Cu2 Br2 122.45(3) 7_565 . ?
Br2 Cu2 Br1 111.92(2) 7_565 . ?
Br2 Cu2 Br1 103.02(2) . . ?
Br2 Cu2 Br1 101.62(2) 7_565 7_565 ?
Br2 Cu2 Br1 108.96(2) . 7_565 ?
Br1 Cu2 Br1 108.40(2) . 7_565 ?
C1 O1 H1O 114(2) . . ?
C1 N1 C3 120.6(3) . . ?
C1 N1 C2 121.4(3) . . ?
C3 N1 C2 117.8(3) . . ?
O1 C1 N1 121.8(4) . . ?
O1 C1 H1 119.1 . . ?
N1 C1 H1 119.1 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
Br1 Cu1 2.5031(6) . ?
Br1 Cu2 2.6082(7) . ?
Br1 Cu2 2.6563(7) 7_566 ?
Br2 Cu2 2.3948(6) . ?
Cu1 Cu2 2.8461(6) . ?
O1 C1 1.274(5) . ?
O1 H1O 1.214(6) . ?
N1 C1 1.305(5) . ?
N1 C3 1.459(5) . ?
N1 C2 1.464(5) . ?
C1 H1 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
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
C3 N1 C1 O1 177.7(3) . . . . ?
C2 N1 C1 O1 4.0(6) . . . . ?
