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#$Date: 2016-03-26 21:42:58 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180481 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/50/7215071.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_7215071
loop_
_publ_author_name
'Sánchez-Andújar, M.'
'Gómez-Aguirre, L. C.'
'Pato Doldán, B.'
'Yáñez-Vilar, S.'
'Artiaga, R.'
'Llamas-Saiz, A. L.'
'Manna, R. S.'
'Schnelle, F.'
'Lang, M.'
'Ritter, F.'
'Haghighirad, A. A.'
'Señarís-Rodríguez, M. A.'
_publ_section_title
;
 First-order structural transition in the multiferroic perovskite-like
 formate [(CH3)2NH2][Mn(HCOO)3]
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              3558
_journal_paper_doi               10.1039/c3ce42411a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.750(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3644(17)
_cell_length_b                   8.3180(10)
_cell_length_c                   8.8927(11)
_cell_measurement_temperature    185(2)
_cell_volume                     913.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEXII area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4783
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.445
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4776
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(7)
_refine_ls_extinction_coef       0.028(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   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         4783
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0948P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                3060
_reflns_number_total             4783
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3ce42411a2.cif
_cod_data_source_block           ja12bpd1n
_cod_original_cell_volume        913.14(19)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7215071
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn1 Mn 0.0000 0.25159(15) 0.0000 0.0149(2) Uani 1 1 d U
O1 O 0.1597(5) 0.1451(8) 0.1658(10) 0.0240(16) Uani 1 1 d U
O2 O 0.0476(6) 0.5210(7) -0.3603(10) 0.0282(18) Uani 1 1 d U
O3 O 0.0492(5) 0.3373(8) -0.1791(10) 0.0256(17) Uani 1 1 d U
O4 O -0.0528(6) -0.0272(7) 0.3561(9) 0.0233(16) Uani 1 1 d U
O5 O -0.0522(5) 0.1614(7) 0.1783(9) 0.0208(15) Uani 1 1 d U
C21 C -0.3041(10) 0.2692(10) 0.0975(17) 0.034(3) Uani 1 1 d U
H21A H -0.3046 0.1561 0.0661 0.051 Uiso 1 1 calc R
H21B H -0.3117 0.3380 0.0024 0.051 Uiso 1 1 calc R
H21C H -0.3645 0.2891 0.1167 0.051 Uiso 1 1 calc R
C1 C 0.2496(11) 0.2131(6) 0.251(2) 0.0205(11) Uani 1 1 d U
H1 H 0.2505 0.3273 0.2528 0.025 Uiso 1 1 calc R
O11 O 0.3383(5) 0.1421(7) 0.3342(10) 0.0234(16) Uani 1 1 d U
C3 C 0.0348(7) 0.4743(12) -0.2411(16) 0.021(2) Uani 1 1 d U
H3 H 0.0110 0.5528 -0.1905 0.025 Uiso 1 1 calc R
C4 C -0.0250(8) 0.0272(12) 0.2548(16) 0.022(2) Uani 1 1 d U
H4 H 0.0209 -0.0384 0.2330 0.026 Uiso 1 1 calc R
N22 N -0.1969(5) 0.3072(6) 0.2654(10) 0.0300(13) Uani 1 1 d U
H22A H -0.1405 0.2614 0.2597 0.036 Uiso 1 1 calc R
H22B H -0.1863 0.4167 0.2758 0.036 Uiso 1 1 calc R
C23 C -0.1981(10) 0.2454(9) 0.4185(18) 0.036(3) Uani 1 1 d U
H23A H -0.1299 0.2733 0.5248 0.054 Uiso 1 1 calc R
H23B H -0.2063 0.1283 0.4097 0.054 Uiso 1 1 calc R
H23C H -0.2587 0.2933 0.4236 0.054 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
O3 Mn1 O4 89.8(3) . 2_554
O3 Mn1 O2 90.5(3) . 2_565
O4 Mn1 O2 178.2(4) 2_554 2_565
O3 Mn1 O1 90.3(3) . .
O4 Mn1 O1 88.8(3) 2_554 .
O2 Mn1 O1 93.0(3) 2_565 .
O3 Mn1 O11 90.3(3) . 4_454
O4 Mn1 O11 91.1(3) 2_554 4_454
O2 Mn1 O11 87.1(3) 2_565 4_454
O1 Mn1 O11 179.4(4) . 4_454
O3 Mn1 O5 178.9(3) . .
O4 Mn1 O5 89.2(2) 2_554 .
O2 Mn1 O5 90.5(2) 2_565 .
O1 Mn1 O5 90.1(2) . .
O11 Mn1 O5 89.3(2) 4_454 .
C1 O1 Mn1 129.0(6) . .
C3 O2 Mn1 128.8(6) . 2_564
C3 O3 Mn1 126.0(6) . .
C4 O4 Mn1 126.6(6) . 2
C4 O5 Mn1 124.3(6) . .
N22 C21 H21A 109.5 . .
N22 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
N22 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O11 C1 O1 124.8(5) . .
O11 C1 H1 117.6 . .
O1 C1 H1 117.6 . .
C1 O11 Mn1 127.9(6) . 4
O2 C3 O3 127.7(9) . .
O2 C3 H3 116.2 . .
O3 C3 H3 116.2 . .
O4 C4 O5 126.0(8) . .
O4 C4 H4 117.0 . .
O5 C4 H4 117.0 . .
C23 N22 C21 110.5(8) . .
C23 N22 H22A 109.6 . .
C21 N22 H22A 109.6 . .
C23 N22 H22B 109.6 . .
C21 N22 H22B 109.6 . .
H22A N22 H22B 108.1 . .
N22 C23 H23A 109.5 . .
N22 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O3 2.167(7) .
Mn1 O4 2.168(6) 2_554
Mn1 O2 2.173(6) 2_565
Mn1 O1 2.182(6) .
Mn1 O11 2.202(6) 4_454
Mn1 O5 2.204(6) .
O1 C1 1.250(13) .
O2 C3 1.228(12) .
O2 Mn1 2.173(6) 2_564
O3 C3 1.236(12) .
O4 C4 1.242(11) .
O4 Mn1 2.168(6) 2
O5 C4 1.261(12) .
C21 N22 1.533(15) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C1 O11 1.247(13) .
C1 H1 0.9500 .
O11 Mn1 2.202(6) 4
C3 H3 0.9500 .
C4 H4 0.9500 .
N22 C23 1.463(14) .
N22 H22A 0.9200 .
N22 H22B 0.9200 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 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_4
O3 Mn1 O1 C1 64.9(11) . .
O4 Mn1 O1 C1 154.7(11) 2_554 .
O2 Mn1 O1 C1 -25.6(11) 2_565 .
O11 Mn1 O1 C1 -124(37) 4_454 .
O5 Mn1 O1 C1 -116.1(10) . .
O4 Mn1 O3 C3 138.3(8) 2_554 .
O2 Mn1 O3 C3 -39.9(9) 2_565 .
O1 Mn1 O3 C3 -132.9(8) . .
O11 Mn1 O3 C3 47.2(8) 4_454 .
O5 Mn1 O3 C3 114(17) . .
O3 Mn1 O5 C4 76(17) . .
O4 Mn1 O5 C4 51.2(8) 2_554 .
O2 Mn1 O5 C4 -130.6(8) 2_565 .
O1 Mn1 O5 C4 -37.6(8) . .
O11 Mn1 O5 C4 142.3(8) 4_454 .
Mn1 O1 C1 O11 -175.2(8) . .
O1 C1 O11 Mn1 -176.3(8) . 4
Mn1 O2 C3 O3 169.4(7) 2_564 .
Mn1 O3 C3 O2 -169.0(7) . .
Mn1 O4 C4 O5 -176.4(7) 2 .
Mn1 O5 C4 O4 179.9(7) . .
