#------------------------------------------------------------------------------
#$Date: 2023-05-11 00:44:56 +0200 (Thu 11 de May de 2023) $
#$Revision: 283661 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/29/7712996.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_7712996
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         'Br2 Cu, C H6 N'
_chemical_formula_sum            'C H6 Br2 Cu N'
_chemical_formula_weight         255.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_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                 114.5389(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6073(8)
_cell_length_b                   5.4260(3)
_cell_length_c                   8.3933(5)
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.60
_cell_measurement_theta_min      4.10
_cell_volume                     563.73(6)
_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 0.977
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-III area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9622
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.596
_diffrn_reflns_theta_min         4.101
_exptl_absorpt_coefficient_mu    17.891
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.097
_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    3.010
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0090(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         1110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0165P)²+1.3P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1078
_reflns_number_total             1110
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt00687e2.cif
_cod_data_source_block           MACuBr2
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7712996
_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   0.099
_shelx_estimated_absorpt_t_max   0.413
_shelxl_version_number           2013-4
_shelx_res_file
; 
TITL MA112 in C2/m 
CELL  0.71073  13.6073   5.4260   8.3933   90.0000  114.5389  90.0000 
ZERR    4.000   0.0008   0.0003   0.0005    0.0000    0.0015   0.0000 
LATT  7 
SYMM -X, Y, -Z 
SFAC C H BR CU N 
UNIT 4 24 8 4 4 
TEMP -173.0 
SIZE 0.06 0.09 0.24 
  
L.S. 24 
BOND $H 
ACTA 
EQIV $3 -x+3/2, -y+3/2, -z+1 
HTAB N1 Br2_$3 
HTAB N1 Br1 
EQIV $4 -x+3/2, -y+1/2, -z+1 
HTAB N1 Br2_$4 
EQIV $5 x, y+1, z 
HTAB N1 Br1_$5 
  
WGHT    0.016500    1.300000 
EXTI    0.009043 
FVAR       0.51096 
BR1   3    0.520312    0.000000    0.263904    10.50000    0.02128    0.01354 = 
         0.01810    0.00000    0.01325    0.00000 
BR2   3    0.664985    0.500000    0.646802    10.50000    0.01105    0.01667 = 
         0.01548    0.00000    0.00520    0.00000 
CU1   4    0.500000    0.243159    0.500000    10.50000    0.01739    0.01530 = 
         0.01971    0.00000    0.00988    0.00000 
N1    5    0.676211    0.500000    0.258206    10.50000    0.02768    0.01661 = 
         0.01948    0.00000    0.01489    0.00000 
AFIX 137 
PART  -1 
H1D   2    0.735690    0.590975    0.322778    10.50000   -1.50000 
H1E   2    0.684633    0.343950    0.301607    10.50000   -1.50000 
H1F   2    0.616842    0.569667    0.263624    10.50000   -1.50000 
AFIX   0 
C1    1    0.662266    0.492493    0.072883    10.50000    0.02951    0.02395 = 
         0.01634    0.00587    0.01115    0.00332 
AFIX 137 
H1A   2    0.604148    0.605249    0.002560    10.50000   -1.50000 
H1B   2    0.643731    0.324489    0.027394    10.50000   -1.50000 
H1C   2    0.729732    0.542796    0.066581    10.50000   -1.50000 
PART   0 
  
AFIX   0 
HKLF 4 
  
REM  MA112 in C2/m 
REM R1 =  0.0169 for    1078 Fo > 4sig(Fo)  and  0.0177 for all    1110 data 
REM     36 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0165      0.7184 
  
REM Highest difference peak  0.625,  deepest hole -0.706,  1-sigma level  0.121 
Q1    1   0.6646  0.6352  0.6423  11.00000  0.05    0.62 
Q2    1   0.5201 -0.1374  0.2620  11.00000  0.05    0.60 
Q3    1   0.6889  0.5000  0.7444  10.50000  0.05    0.54 
Q4    1   0.5467  0.0000  0.3523  10.50000  0.05    0.48 
Q5    1   0.4756  0.2790  0.4021  11.00000  0.05    0.44 
Q6    1   0.6471  0.5000  0.4424  10.50000  0.05    0.43 
Q7    1   0.4990  0.0000  0.1591  10.50000  0.05    0.42 
Q8    1   0.6665  0.5000  0.1585  10.50000  0.05    0.38 
Q9    1   0.4444  0.0000  0.3564  10.50000  0.05    0.36 
Q10   1   0.7495  0.5000  0.5394  10.50000  0.05    0.36 
Q11   1   0.5000  0.3890  0.5000  10.50000  0.05    0.34 
Q12   1   0.5958  0.6326  0.4035  11.00000  0.05    0.33 
Q13   1   0.4364  0.3451  0.3037  11.00000  0.05    0.31 
Q14   1   0.4292  0.2436  0.6021  11.00000  0.05    0.31 
Q15   1   0.6433  0.5000  0.5417  10.50000  0.05    0.30 
Q16   1   0.5000  0.0966  0.5000  10.50000  0.05    0.27 
Q17   1   0.6909  0.2445  0.4207  11.00000  0.05    0.27 
Q18   1   0.7104  0.7210  0.7594  11.00000  0.05    0.27 
Q19   1   0.4108  0.0979  0.4149  11.00000  0.05    0.27 
Q20   1   0.6468  0.2301 -0.1152  11.00000  0.05    0.27 
;
_shelx_res_checksum              89143
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.52031(2) 0.0000 0.26390(3) 0.01594(7) Uani 1 2 d S T P . .
Br2 Br 0.66498(2) 0.5000 0.64680(3) 0.01450(7) Uani 1 2 d S T P . .
Cu1 Cu 0.5000 0.24316(5) 0.5000 0.01674(8) Uani 1 2 d S T P . .
N1 N 0.67621(18) 0.5000 0.2582(3) 0.0196(4) Uani 1 2 d S T P . .
H1D H 0.7357 0.5910 0.3228 0.029 Uiso 0.5 1 calc R U P A -1
H1E H 0.6846 0.3440 0.3016 0.029 Uiso 0.5 1 calc R U P A -1
H1F H 0.6168 0.5697 0.2636 0.029 Uiso 0.5 1 calc R U P A -1
C1 C 0.6623(3) 0.492(6) 0.0729(4) 0.0227(12) Uani 0.5 1 d . . P B -1
H1A H 0.6041 0.6052 0.0026 0.034 Uiso 0.5 1 calc R U P B -1
H1B H 0.6437 0.3245 0.0274 0.034 Uiso 0.5 1 calc R U P B -1
H1C H 0.7297 0.5428 0.0666 0.034 Uiso 0.5 1 calc R U P B -1
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 0.02128(11) 0.01354(11) 0.01810(11) 0.000 0.01325(8) 0.000
Br2 0.01105(10) 0.01667(11) 0.01548(10) 0.000 0.00520(7) 0.000
Cu1 0.01739(13) 0.01530(13) 0.01971(13) 0.000 0.00988(10) 0.000
N1 0.0277(9) 0.0166(8) 0.0195(8) 0.000 0.0149(7) 0.000
C1 0.0295(12) 0.024(3) 0.0163(10) 0.006(5) 0.0111(9) 0.003(5)
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_
_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 64.001(13) . 5_656 ?
Cu1 Br2 Cu1 68.051(13) 5_666 . ?
Br1 Cu1 Br1 116.000(13) 5_656 . ?
Br1 Cu1 Br2 106.140(7) 5_656 . ?
Br1 Cu1 Br2 108.365(7) . . ?
Br1 Cu1 Br2 108.364(7) 5_656 5_666 ?
Br1 Cu1 Br2 106.141(7) . 5_666 ?
Br2 Cu1 Br2 111.949(13) . 5_666 ?
Br1 Cu1 Cu1 58.000(6) 5_656 5_656 ?
Br1 Cu1 Cu1 58.000(6) . 5_656 ?
Br2 Cu1 Cu1 124.026(6) . 5_656 ?
Br2 Cu1 Cu1 124.025(6) 5_666 5_656 ?
Br1 Cu1 Cu1 122.000(6) 5_656 5_666 ?
Br1 Cu1 Cu1 122.000(6) . 5_666 ?
Br2 Cu1 Cu1 55.974(6) . 5_666 ?
Br2 Cu1 Cu1 55.975(6) 5_666 5_666 ?
Cu1 Cu1 Cu1 180.0 5_656 5_666 ?
C1 N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1F 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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 2.4898(2) . ?
Br1 Cu1 2.4898(2) 5_656 ?
Br2 Cu1 2.4905(2) 5_666 ?
Br2 Cu1 2.4905(2) . ?
Cu1 Br1 2.4898(2) 5_656 ?
Cu1 Br2 2.4906(2) 5_666 ?
Cu1 Cu1 2.6388(6) 5_656 ?
Cu1 Cu1 2.7872(6) 5_666 ?
N1 C1 1.487(4) . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N1 H1F 0.9100 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
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 H1D Br2 0.91 2.56 3.3518(13) 146.4 7_666
N1 H1E Br1 0.91 2.83 3.4565(13) 127.4 .
N1 H1E Br2 0.91 2.67 3.3518(13) 132.5 7_656
N1 H1F Br1 0.91 2.68 3.4565(13) 143.9 1_565
