#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:13:23 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179367 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/64/4326427.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_4326427
loop_
_publ_author_name
'M. Sánchez-Andújar'
'S. Presedo'
'S. Yáñez-Vilar'
'S. Castro-García'
'J. Shamir'
'M. A. Señarís-Rodríguez'
_publ_contact_author_address
;Universidad A Coruna
Facultad de Ciencias
Campus da Zapateira
15071 A Coruna (Spain)
;
_publ_contact_author_email       tonasr@udc.es
_publ_contact_author_fax         '+34 981167065'
_publ_contact_author_name        'M.A. Senaris-R'
_publ_contact_author_phone       '+34 981167000'
_publ_section_title
;
 Correction to Characterization of the Order-Disorder Dielectric
 Transition in the Hybrid Organic-Inorganic Perovskite-like Formate
 Mn(HCOO)3[(CH3)2NH2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9734
_journal_page_last               9734
_journal_paper_doi               10.1021/ic201638t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C5 H11 Mn N O6'
_chemical_formula_weight         236.09
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   8.3371(8)
_cell_length_b                   8.3371(8)
_cell_length_c                   22.909(5)
_cell_measurement_reflns_used    1097
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.322
_cell_measurement_theta_min      3.33335
_cell_volume                     1379.0(4)
_computing_cell_refinement       'SAINT V7.12A Bruker Nonius 2004'
_computing_data_collection       'Apex2 V.1.0-27 Bruker Nonius 2005'
_computing_data_reduction        'SAINT & XPREP V.6.14 2003 Bruker-AXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEXII area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            4154
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.9188
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS: Area-Detector Absorption Correction. Bruker-AXS
  Release 2004/1, in Apex2 suite package, (2004).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       prism
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0065(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0288
_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)+(0.0404P)²+1.9843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                323
_reflns_number_total             380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201638t_si_001_2.cif
_cod_data_source_block           Mn(CHOO)3-NH2(CH3)2_room_temperature
_cod_original_cell_volume        1379.0(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4326427
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
C1 C 0.2153(4) 0.8820(4) 0.0833 0.0303(7) Uani 1 2 d S
C2 C 0.3333 0.6667 -0.0296(2) 0.0591(14) Uani 1 3 d S
N1 N 0.4209(11) 0.6667 -0.0833 0.048(2) Uani 0.33 2 d SP
H1 H 0.103(5) 0.769(5) 0.0833 0.037(9) Uiso 1 2 d S
Mn1 Mn 0.0000 1.0000 0.0000 0.0214(3) Uani 1 6 d S
O1 O 0.2208(2) 1.0105(2) 0.05443(7) 0.0373(5) Uani 1 1 d .
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
C1 0.0275(11) 0.0275(11) 0.0355(18) 0.0010(6) -0.0010(6) 0.0133(12)
C2 0.070(2) 0.070(2) 0.038(3) 0.000 0.000 0.0348(11)
N1 0.030(3) 0.025(4) 0.086(7) -0.008(4) -0.004(2) 0.013(2)
Mn1 0.0216(3) 0.0216(3) 0.0212(5) 0.000 0.000 0.01079(17)
O1 0.0339(9) 0.0348(9) 0.0424(10) 0.0070(7) -0.0084(7) 0.0166(7)
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'
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'
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
O1 C1 O1 126.5(3) . 16_454
O1 C1 H1 116.75(15) . .
O1 C1 H1 116.75(15) 16_454 .
N1 C2 N1 52.4(6) 2_665 3_565
N1 C2 N1 52.4(6) 2_665 .
N1 C2 N1 52.4(6) 3_565 .
N1 N1 N1 60.000(1) 3_565 2_665
N1 N1 C2 63.8(3) 3_565 10_454
N1 N1 C2 63.8(3) 2_665 10_454
N1 N1 C2 63.8(3) 3_565 .
N1 N1 C2 63.8(3) 2_665 .
C2 N1 C2 118.7(7) 10_454 .
O1 Mn1 O1 180.0 . 19_575
O1 Mn1 O1 89.25(6) . 20_455
O1 Mn1 O1 90.75(6) 19_575 20_455
O1 Mn1 O1 90.75(6) . 2_675
O1 Mn1 O1 89.25(6) 19_575 2_675
O1 Mn1 O1 180.00(7) 20_455 2_675
O1 Mn1 O1 89.25(6) . 21_665
O1 Mn1 O1 90.75(6) 19_575 21_665
O1 Mn1 O1 90.75(6) 20_455 21_665
O1 Mn1 O1 89.25(6) 2_675 21_665
O1 Mn1 O1 90.75(6) . 3_465
O1 Mn1 O1 89.25(6) 19_575 3_465
O1 Mn1 O1 89.25(6) 20_455 3_465
O1 Mn1 O1 90.75(6) 2_675 3_465
O1 Mn1 O1 180.0 21_665 3_465
C1 O1 Mn1 127.05(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.241(2) .
C1 O1 1.241(2) 16_454
C1 H1 0.94(4) .
C2 N1 1.431(7) 2_665
C2 N1 1.431(7) 3_565
C2 N1 1.431(7) .
N1 N1 1.264(16) 3_565
N1 N1 1.264(16) 2_665
N1 C2 1.431(7) 10_454
Mn1 O1 2.1885(15) .
Mn1 O1 2.1885(15) 19_575
Mn1 O1 2.1885(15) 20_455
Mn1 O1 2.1885(15) 2_675
Mn1 O1 2.1885(15) 21_665
Mn1 O1 2.1885(15) 3_465
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
N1 C2 N1 N1 -67.74(18) 2_665 3_565
N1 C2 N1 N1 67.74(18) 3_565 2_665
N1 C2 N1 C2 -33.87(9) 2_665 10_454
N1 C2 N1 C2 33.87(9) 3_565 10_454
O1 C1 O1 Mn1 176.96(16) 16_454 .
O1 Mn1 O1 C1 -108(18) 19_575 .
O1 Mn1 O1 C1 -61.49(10) 20_455 .
O1 Mn1 O1 C1 118.51(10) 2_675 .
O1 Mn1 O1 C1 -152.25(16) 21_665 .
O1 Mn1 O1 C1 27.75(16) 3_465 .
