#------------------------------------------------------------------------------
#$Date: 2023-05-11 01:44:56 +0300 (Thu, 11 May 2023) $
#$Revision: 283661 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712994.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_7712994
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         'Br3 Cu2, C H6 N'
_chemical_formula_sum            'C H6 Br3 Cu2 N'
_chemical_formula_weight         398.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2023-03-20 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.383(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4716(6)
_cell_length_b                   5.5703(3)
_cell_length_c                   8.4791(9)
_cell_measurement_reflns_used    2792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.34
_cell_measurement_theta_min      2.57
_cell_volume                     369.98(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_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 0.969
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3408
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.986
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    21.836
_exptl_absorpt_correction_T_max  0.077
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.580
_exptl_crystal_description       prism
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.248
_refine_diff_density_min         -2.932
_refine_diff_density_rms         0.550
_refine_ls_extinction_coef       0.019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0690
_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)+(0.0898P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                975
_reflns_number_total             1111
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00687e2.cif
_cod_data_source_block           MACu2Br3
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7712994
_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   0.091
_shelx_estimated_absorpt_t_max   0.197
_shelxl_version_number           2013-4
_shelx_res_file
;
TITL MACu2Br3 in P2(1)/m
CELL 0.71073   8.4716   5.5703   8.4791  90.000 112.383  90.000
ZERR    2.00   0.0006   0.0003   0.0009   0.000   0.010   0.000
LATT 1
SYMM -X, 0.5+Y, -Z
SFAC C H N Cu Br
UNIT 2 12 2 4 6
TEMP -173.0
SIZE 0.11 0.12 0.21

OMIT -2 60
OMIT    -4   0   2
L.S. 12
BOND $H
ACTA
CONF
EQIV $1 -x+1, -y, -z+1
HTAB N1 Br1_$1
EQIV $2 x, y-1, z
HTAB N1 Br2_$2
EQIV $3 -x+2, -y+1, -z+1
HTAB N1 Br2_$3

WGHT    0.089800
EXTI    0.018670
FVAR       0.42974
BR1   5    0.599998    0.250000    0.718671    10.50000    0.00848    0.01234 =
         0.01561    0.00000    0.00457    0.00000
BR2   5    0.890301    0.750000    0.586473    10.50000    0.01241    0.01212 =
         0.01352    0.00000    0.00599    0.00000
BR3   5    0.872695    0.750000    1.067421    10.50000    0.00894    0.01272 =
         0.01256    0.00000    0.00346    0.00000
CU1   4    0.854512    0.502781    0.808621    11.00000    0.01471    0.01545 =
         0.01996    0.00026    0.00675   -0.00267
N1    3    0.681707    0.250000    0.355111    10.50000    0.01606    0.02688 =
         0.01054    0.00000    0.00392    0.00000
AFIX   3
H1A   2    0.633677    0.120660    0.382411    11.00000   -1.50000
H1B   2    0.796257    0.250000    0.406941    10.50000   -1.50000
AFIX   0
C1    1    0.624840    0.250000    0.168456    10.50000    0.01776    0.01911 =
         0.01496    0.00000    0.00302    0.00000
AFIX   3
H1C   2    0.673350    0.111490    0.136596    11.00000   -1.50000
H1D   2    0.500890    0.250000    0.098136    10.50000   -1.50000

AFIX   0
HKLF 4

REM  MACu2Br3 in P2(1)/m
REM R1 =  0.0690 for     975 Fo > 4sig(Fo)  and  0.0731 for all    1111 data
REM     41 parameters refined using      0 restraints

END

WGHT      0.0898      0.0000

REM Highest difference peak  2.248,  deepest hole -2.932,  1-sigma level  0.550
Q1    1   0.8274  0.6031  0.8174  11.00000  0.05    2.25
Q2    1   0.8729  0.9420  1.0781  11.00000  0.05    1.97
Q3    1   1.0219  0.7500  0.7605  10.50000  0.05    1.90
Q4    1   0.9007  0.9226  0.6021  11.00000  0.05    1.86
Q5    1   0.9082  0.3998  0.7157  11.00000  0.05    1.84
Q6    1   0.5925  0.0638  0.7171  11.00000  0.05    1.83
Q7    1   0.6348  0.1654  0.7072  11.00000  0.05    1.82
Q8    1   0.8176  0.6497  0.9044  11.00000  0.05    1.75
Q9    1   0.5148  0.2500  0.5007  10.50000  0.05    1.68
Q10   1   0.9087  0.9607  0.9893  11.00000  0.05    1.57
Q11   1   0.8872  0.8447  0.7131  11.00000  0.05    1.57
Q12   1   0.8258  0.8404  1.0736  11.00000  0.05    1.52
Q13   1   0.7477  0.8368  0.5137  11.00000  0.05    1.47
Q14   1   0.7675  0.2500  0.9068  10.50000  0.05    1.46
Q15   1   0.6942  0.7500  0.6370  10.50000  0.05    1.45
Q16   1   0.9594  0.7500  1.2691  10.50000  0.05    1.45
Q17   1   0.9140  0.9595  0.4986  11.00000  0.05    1.42
Q18   1   0.8765  0.3661  0.8180  11.00000  0.05    1.41
Q19   1   0.7158  0.7500  0.8771  10.50000  0.05    1.35
Q20   1   0.7426  0.4660  0.6553  11.00000  0.05    1.35
;
_shelx_res_checksum              34674
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.60000(11) 0.2500 0.71867(12) 0.0121(3) Uani 1 2 d S T P . .
Br2 Br 0.89030(12) 0.7500 0.58647(12) 0.0124(3) Uani 1 2 d S T P . .
Br3 Br 0.87269(11) 0.7500 1.06742(11) 0.0116(3) Uani 1 2 d S T P . .
Cu1 Cu 0.85451(11) 0.50278(14) 0.80862(12) 0.0167(3) Uani 1 1 d . . . . .
N1 N 0.6817(11) 0.2500 0.3551(11) 0.0182(16) Uani 1 2 d S T P . .
H1A H 0.6337 0.1207 0.3824 0.027 Uiso 1 1 d R U . . .
H1B H 0.7963 0.2500 0.4069 0.027 Uiso 1 2 d R U P . .
C1 C 0.6248(12) 0.2500 0.1685(12) 0.018(2) Uani 1 2 d S T P . .
H1C H 0.6734 0.1115 0.1366 0.027 Uiso 1 1 d R U . . .
H1D H 0.5009 0.2500 0.0981 0.027 Uiso 1 2 d R U P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0085(5) 0.0123(4) 0.0156(5) 0.000 0.0046(4) 0.000
Br2 0.0124(5) 0.0121(4) 0.0135(5) 0.000 0.0060(4) 0.000
Br3 0.0089(4) 0.0127(5) 0.0126(6) 0.000 0.0035(4) 0.000
Cu1 0.0147(5) 0.0155(5) 0.0200(6) 0.0003(3) 0.0067(4) -0.0027(3)
N1 0.016(4) 0.027(4) 0.011(4) 0.000 0.004(3) 0.000
C1 0.018(5) 0.019(5) 0.015(5) 0.000 0.003(4) 0.000
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'
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_
_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 70.44(4) . 4_565 ?
Cu1 Br2 Cu1 68.60(4) . 4_575 ?
Cu1 Br3 Cu1 65.51(4) 4_575 . ?
Cu1 Br3 Cu1 78.79(4) 4_575 2_757 ?
Cu1 Br3 Cu1 113.55(4) . 2_757 ?
Cu1 Br3 Cu1 113.55(4) 4_575 3_767 ?
Cu1 Br3 Cu1 78.79(4) . 3_767 ?
Cu1 Br3 Cu1 66.60(4) 2_757 3_767 ?
Br1 Cu1 Br2 115.99(5) . . ?
Br1 Cu1 Br3 109.74(4) . . ?
Br2 Cu1 Br3 112.03(3) . . ?
Br1 Cu1 Br3 111.23(3) . 3_767 ?
Br2 Cu1 Br3 105.57(4) . 3_767 ?
Br3 Cu1 Br3 101.21(4) . 3_767 ?
Br1 Cu1 Cu1 125.22(2) . 4_575 ?
Br2 Cu1 Cu1 55.70(2) . 4_575 ?
Br3 Cu1 Cu1 57.24(2) . 4_575 ?
Br3 Cu1 Cu1 123.30(2) 3_767 4_575 ?
Br1 Cu1 Cu1 54.78(2) . 4_565 ?
Br2 Cu1 Cu1 124.30(2) . 4_565 ?
Br3 Cu1 Cu1 122.76(2) . 4_565 ?
Br3 Cu1 Cu1 56.70(2) 3_767 4_565 ?
Cu1 Cu1 Cu1 180.00(7) 4_575 4_565 ?
C1 N1 H1A 106.4 . . ?
C1 N1 H1B 112.1 . . ?
H1A N1 H1B 112.5 . . ?
N1 C1 H1C 107.7 . . ?
N1 C1 H1D 119.1 . . ?
H1C C1 H1D 107.4 . . ?
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 2.4415(11) . ?
Br1 Cu1 2.4415(11) 4_565 ?
Br2 Cu1 2.4436(10) . ?
Br2 Cu1 2.4436(10) 4_575 ?
Br3 Cu1 2.5452(12) 4_575 ?
Br3 Cu1 2.5452(12) . ?
Br3 Cu1 2.5648(11) 2_757 ?
Br3 Cu1 2.5648(11) 3_767 ?
Cu1 Br3 2.5648(11) 3_767 ?
Cu1 Cu1 2.7542(16) 4_575 ?
Cu1 Cu1 2.8161(16) 4_565 ?
N1 C1 1.468(12) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9906 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br1 0.90 2.76 3.565(5) 149.3 3_656
N1 H1B Br2 0.90 2.63 3.468(9) 154.3 3_766
