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#$Date: 2017-06-03 05:17:50 +0300 (Sat, 03 Jun 2017) $
#$Revision: 197189 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/32/7043201.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_7043201
loop_
_publ_author_name
'maczka, miroslaw'
'Janczak, Jan'
'Trzebiatowska, Monika'
'Sieradzki, Adam'
'Pawlus, Sebastian'
'Pikul, Adam'
_publ_section_title
;
 Synthesis and temperature-dependent studies of perovskite-like manganese
 formate framework templated by protonated acetamidine
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01251A
_journal_year                    2017
_chemical_formula_moiety         'C3 H3 Mn O6, C2 H7 N2'
_chemical_formula_sum            'C5 H10 Mn N2 O6'
_chemical_formula_weight         249.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-31 deposited with the CCDC.
2017-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7482(17)
_cell_length_b                   12.089(2)
_cell_length_c                   9.0317(18)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.82
_cell_volume                     955.2(3)
_computing_cell_refinement
;
CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlis CCD 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlis Red 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      320(2)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'KUMA KM-4 with CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20981
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.543
_diffrn_reflns_theta_min         2.815
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      1.73
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0315
_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)+(0.0608P)²+0.7230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                621
_reflns_number_total             721
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01251a2.cif
_cod_data_source_block           mn330
_cod_original_cell_volume        955.1(3)
_cod_database_code               7043201
_shelx_shelxl_version_number     2014/7
_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   0.368
_shelx_estimated_absorpt_t_max   0.769
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-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_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
Mn Mn 0.0000 0.5000 0.5000 0.02407(19) Uani 1 4 d S T P . .
O1 O 0.0000 0.65833(14) 0.38771(19) 0.0501(5) Uani 1 2 d S T P . .
O2 O 0.17145(19) 0.43787(12) 0.34529(15) 0.0563(4) Uani 1 1 d . . . . .
C1 C 0.0000 0.7500 0.4448(4) 0.0454(9) Uani 1 4 d S T P . .
H1 H 0.0000 0.7500 0.5478 0.055 Uiso 1 4 calc R U P . .
C2 C 0.2500 0.4730(2) 0.2500 0.0570(8) Uani 1 2 d S T P . .
H2 H 0.2500 0.5500 0.2500 0.068 Uiso 1 2 calc R U P . .
N1 N 0.0000 0.2500 0.1594(4) 0.0574(10) Uani 1 4 d S T P A .
H1N H 0.0000 0.316(4) 0.190(4) 0.069 Uiso 1 2 d S U P . .
C3 C 0.0000 0.2500 0.0144(4) 0.0486(10) Uani 1 4 d S T P . .
C4 C -0.101(3) 0.312(3) -0.075(3) 0.069(8) Uani 0.25 1 d . . P A -1
H4A H -0.1724 0.2628 -0.1225 0.103 Uiso 0.25 1 calc R U P A -1
H4B H -0.0441 0.3512 -0.1492 0.103 Uiso 0.25 1 calc R U P A -1
H4C H -0.1561 0.3638 -0.0148 0.103 Uiso 0.25 1 calc R U P A -1
N2 N -0.082(2) 0.3325(19) -0.053(2) 0.050(4) Uani 0.25 1 d . . P A -2
H2A H -0.1291 0.3806 0.0002 0.060 Uiso 0.25 1 calc R U P A -2
H2B H -0.0852 0.3362 -0.1477 0.060 Uiso 0.25 1 calc R U P A -2
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 Mn O1 180.00(4) . 9_566
O1 Mn O2 90.25(5) . 12
O1 Mn O2 89.75(5) 9_566 12
O1 Mn O2 90.25(5) . .
O1 Mn O2 89.75(5) 9_566 .
O2 Mn O2 86.79(9) 12 .
O1 Mn O2 89.75(5) . 4_566
O1 Mn O2 90.25(5) 9_566 4_566
O2 Mn O2 180.00(5) 12 4_566
O2 Mn O2 93.21(9) . 4_566
O1 Mn O2 89.75(5) . 9_566
O1 Mn O2 90.25(5) 9_566 9_566
O2 Mn O2 93.21(9) 12 9_566
O2 Mn O2 180.00(6) . 9_566
O2 Mn O2 86.79(9) 4_566 9_566
C1 O1 Mn 127.1(2) . .
C2 O2 Mn 137.95(16) . .
O1 C1 O1 130.1(4) 2_565 .
O1 C1 H1 115.0 2_565 .
O1 C1 H1 115.0 . .
O2 C2 O2 137.8(3) 7_545 .
O2 C2 H2 111.1 7_545 .
O2 C2 H2 111.1 . .
C3 N1 H1N 109(3) . .
N1 C3 N2 116.3(8) . .
N1 C3 C4 124.9(11) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 N2 H2A 120.0 . .
C3 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn O1 2.1661(17) .
Mn O1 2.1661(17) 9_566
Mn O2 2.1831(13) 12
Mn O2 2.1831(13) .
Mn O2 2.1831(13) 4_566
Mn O2 2.1831(13) 9_566
O1 C1 1.222(2) .
O2 C2 1.1806(17) .
C1 O1 1.222(2) 2_565
C1 H1 0.9300 .
C2 O2 1.1806(17) 7_545
C2 H2 0.9300 .
N1 C3 1.310(5) .
N1 H1N 0.85(4) .
C3 N2 1.37(2) .
C3 C4 1.41(2) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
N2 H2A 0.8600 .
N2 H2B 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 H1N O2 0.85(4) 2.52(3) 3.198(2) 137.1(17) .
N1 H1N O2 0.85(4) 2.52(3) 3.198(2) 137.1(17) 12
N2 H2A O2 0.86 2.34 3.131(19) 153.1 14_455
N2 H2B O1 0.86 2.29 3.111(18) 158.8 9_565
