#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:33:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179485 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/82/4338267.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_4338267
loop_
_publ_author_name
'Mączka, Mirosław'
'Ciupa, Aneta'
'Gągor, Anna'
'Sieradzki, Adam'
'Pikul, Adam'
'Macalik, Bogusław'
'Drozd, Marek'
_publ_section_title
;
 Perovskite Metal Formate Framework of [NH2-CH(+)-NH2]Mn(HCOO)3]: Phase
 Transition, Magnetic, Dielectric, and Phonon Properties.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5260
_journal_page_last               5268
_journal_paper_doi               10.1021/ic500479e
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C4 H8 Mn N2 O6'
_chemical_formula_weight         235.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 119.664(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8035(7)
_cell_length_b                   8.6913(4)
_cell_length_c                   8.4626(4)
_cell_measurement_reflns_used    1067
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      4.55
_cell_volume                     882.20(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.979
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5358
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         4.55
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0068(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1067
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0274
_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)+(0.0350P)²+0.9000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                932
_reflns_number_total             1067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500479e_si_003.cif
_cod_data_source_block           c2c
_cod_depositor_comments
'Adding full bibliography for 4338266--4338268.cif.'
_cod_original_cell_volume        882.20(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4338267
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'
'-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 0.2500 0.2500 0.0000 0.02358(18) Uani 1 2 d S
O1 O 0.18204(12) 0.45814(17) 0.05167(18) 0.0381(4) Uani 1 1 d .
O2 O 0.29546(13) 0.15208(16) 0.26439(18) 0.0379(4) Uani 1 1 d .
O3 O 0.41192(11) 0.36655(17) 0.1399(2) 0.0384(4) Uani 1 1 d .
C1 C 0.5000 0.3013(4) 0.2500 0.0366(6) Uani 1 2 d S
H1 H 0.5000 0.1943 0.2500 0.044 Uiso 1 2 calc SR
C2 C 0.22082(19) 0.5193(2) 0.2025(3) 0.0380(5) Uani 1 1 d .
H2 H 0.2674 0.4587 0.3021 0.046 Uiso 1 1 calc R
N1 N 0.0698(2) 0.8047(3) -0.1041(3) 0.0601(7) Uani 0.90 1 d P
H1A H 0.1148 0.7487 -0.0118 0.072 Uiso 0.90 1 d P
H1B H 0.0732 0.9017 -0.0982 0.072 Uiso 0.90 1 d P
C3 C 0.0000 0.7370(4) -0.2500 0.0519(9) Uani 1 2 d SD
N2 N 0.0000 0.5899(4) -0.2500 0.044(3) Uiso 0.20 2 d SPD
H3A H 0.0460 0.5404 -0.1538 0.053 Uiso 0.20 1 calc PR
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
Mn1 0.0251(2) 0.0212(2) 0.0203(2) -0.00055(12) 0.00803(16) -0.00024(13)
O1 0.0433(8) 0.0341(8) 0.0296(7) -0.0063(5) 0.0125(6) 0.0082(6)
O2 0.0533(9) 0.0293(7) 0.0273(7) 0.0018(5) 0.0170(6) -0.0056(6)
O3 0.0261(7) 0.0334(8) 0.0417(8) 0.0033(6) 0.0062(6) -0.0017(6)
C1 0.0291(14) 0.0276(13) 0.0455(16) 0.000 0.0127(12) 0.000
C2 0.0462(11) 0.0342(11) 0.0251(9) 0.0008(8) 0.0112(8) 0.0130(9)
N1 0.0653(16) 0.0448(13) 0.0385(12) 0.0047(10) 0.0016(11) -0.0020(12)
C3 0.052(2) 0.045(2) 0.0429(19) 0.000 0.0114(16) 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'
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
O2 Mn1 O2 180.00(10) 7 .
O2 Mn1 O1 92.99(5) 7 7
O2 Mn1 O1 87.01(5) . 7
O2 Mn1 O1 87.01(5) 7 .
O2 Mn1 O1 92.99(5) . .
O1 Mn1 O1 180.00(8) 7 .
O2 Mn1 O3 85.83(6) 7 7
O2 Mn1 O3 94.17(6) . 7
O1 Mn1 O3 86.16(6) 7 7
O1 Mn1 O3 93.84(6) . 7
O2 Mn1 O3 94.17(6) 7 .
O2 Mn1 O3 85.83(6) . .
O1 Mn1 O3 93.84(6) 7 .
O1 Mn1 O3 86.16(6) . .
O3 Mn1 O3 180.00(14) 7 .
C2 O1 Mn1 123.76(13) . .
C2 O2 Mn1 127.38(13) 4_545 .
C1 O3 Mn1 123.46(15) . .
O3 C1 O3 125.7(3) 2_655 .
O3 C1 H1 117.1 2_655 .
O3 C1 H1 117.1 . .
O1 C2 O2 127.11(19) . 4
O1 C2 H2 116.4 . .
O2 C2 H2 116.4 4 .
C3 N1 H1A 118.3 . .
C3 N1 H1B 120.8 . .
H1A N1 H1B 120.9 . .
N1 C3 N1 124.9(4) . 2_554
N1 C3 N2 117.53(18) . .
N1 C3 N2 117.53(18) 2_554 .
C3 N2 H3A 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.1759(13) 7
Mn1 O2 2.1759(13) .
Mn1 O1 2.1793(14) 7
Mn1 O1 2.1793(14) .
Mn1 O3 2.1918(14) 7
Mn1 O3 2.1918(14) .
O1 C2 1.233(2) .
O2 C2 1.234(2) 4_545
O3 C1 1.2437(19) .
C1 O3 1.2437(19) 2_655
C1 H1 0.9300 .
C2 O2 1.234(2) 4
C2 H2 0.9300 .
N1 C3 1.273(3) .
N1 H1A 0.8680 .
N1 H1B 0.8445 .
C3 N1 1.273(3) 2_554
C3 N2 1.2788(10) .
N2 H3A 0.8600 .
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 O2 0.87 2.01 2.862(3) 165.4 4
N1 H1B O3 0.84 2.07 2.897(3) 165.3 7_565
N2 H3A O1 0.86 1.96 2.792(2) 163.5 .
