#------------------------------------------------------------------------------
#$Date: 2019-11-23 11:01:46 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 233205 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/56/7235655.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_7235655
loop_
_publ_author_name
'Liu, Jian-Qiang'
'Wu, Jian'
'Wang, Jun'
'Lu, Lu'
'Daiguebonne, Carole'
'Calvez, Guillaume'
'Guillou, Olivier'
'Sakiyama, Hiroshi'
'Weng, Ng Seik'
'Zeller, Matthias'
_publ_section_title
;
 Temperature identification on two 3D Mn(ii) metal--organic frameworks:
 syntheses, adsorption and magnetism
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              20605
_journal_paper_doi               10.1039/c4ra02609h
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C7 H15.33 Mn N O6'
_chemical_formula_weight         264.47
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9042(11)
_cell_length_b                   12.7757(16)
_cell_length_c                   9.2004(11)
_cell_measurement_reflns_used    3700
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.28
_cell_volume                     1046.6(2)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        APEX2
_computing_molecular_graphics    APEX2
_computing_publication_material  APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5038
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.18
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  0.8323
_exptl_absorpt_correction_T_min  0.7174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             549
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.037(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   1.209
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0198
_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)+(0.0262P)²+0.2070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                928
_reflns_number_total             991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra02609h2.cif
_cod_data_source_block           Mn
_cod_database_code               7235655
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.0000 0.5000 0.01657(14) Uani 1 2 d S . .
O1 O 0.29857(9) -0.04201(7) 0.62533(9) 0.0288(2) Uani 1 1 d . . .
O2 O 0.13555(10) -0.04180(7) 0.80773(9) 0.0329(2) Uani 1 1 d . . .
O3 O 0.48286(10) 0.16310(7) 0.58086(10) 0.0314(2) Uani 1 1 d . . .
C1 C 0.25585(12) -0.01780(10) 0.74934(12) 0.0235(3) Uani 1 1 d . . .
H1 H 0.3214 0.0228 0.8043 0.028 Uiso 1 1 calc R . .
C2 C 0.48910(19) 0.2500 0.5247(2) 0.0260(5) Uani 1 2 d S . .
H2A H 0.4098 0.2500 0.4525 0.031 Uiso 0.33(3) 2 calc SPR A 1
H2B H 0.5825 0.2500 0.4705 0.031 Uiso 0.33(3) 2 calc SPR A 1
H2 H 0.5003 0.2500 0.4242 0.031 Uiso 0.67(3) 2 calc SPR A 2
N7 N 1.01193(16) 0.2500 0.50860(15) 0.0259(4) Uani 1 2 d S . .
C4 C 1.0288(3) 0.2500 0.3484(2) 0.0483(6) Uani 1 2 d S . .
H4A H 0.9894 0.3141 0.3096 0.072 Uiso 0.50 1 d PR . .
H4B H 0.9747 0.1918 0.3082 0.072 Uiso 0.50 1 d PR . .
H4C H 1.1332 0.2500 0.3236 0.072 Uiso 1 2 d SR . .
C5 C 1.08389(16) 0.15484(10) 0.56941(15) 0.0396(3) Uani 1 1 d . . .
H5A H 1.0381 0.0937 0.5280 0.059 Uiso 1 1 calc R . .
H5B H 1.0710 0.1539 0.6730 0.059 Uiso 1 1 calc R . .
H5C H 1.1891 0.1554 0.5466 0.059 Uiso 1 1 calc R . .
C6 C 0.8496(2) 0.2500 0.5488(3) 0.0447(5) Uani 1 2 d S . .
H6A H 0.8400 0.2556 0.6525 0.067 Uiso 0.50 1 calc PR . .
H6B H 0.8040 0.1860 0.5165 0.067 Uiso 0.50 1 calc PR . .
H6C H 0.8005 0.3083 0.5034 0.067 Uiso 0.50 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 0.0168(2) 0.0159(2) 0.0170(2) -0.00012(8) 0.00008(8) -0.00016(8)
O1 0.0262(5) 0.0329(5) 0.0272(5) -0.0035(4) 0.0081(3) -0.0046(4)
O2 0.0310(5) 0.0386(5) 0.0291(5) -0.0067(4) 0.0118(4) -0.0044(4)
O3 0.0456(6) 0.0183(5) 0.0304(5) -0.0014(4) 0.0019(4) 0.0005(3)
C1 0.0245(7) 0.0211(6) 0.0249(7) -0.0007(4) -0.0015(6) -0.0016(4)
C2 0.0344(11) 0.0266(12) 0.0169(8) 0.000 0.0008(6) 0.000
N7 0.0292(10) 0.0230(10) 0.0256(10) 0.000 -0.0038(5) 0.000
C4 0.0866(17) 0.0332(12) 0.0251(11) 0.000 -0.0078(10) 0.000
C5 0.0412(8) 0.0369(8) 0.0406(8) 0.0130(6) 0.0043(6) 0.0125(6)
C6 0.0257(10) 0.0345(10) 0.0739(15) 0.000 -0.0056(10) 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
O1 Mn1 O1 180.0 5_656 .
O1 Mn1 O2 88.09(3) 5_656 2_554
O1 Mn1 O2 91.91(3) . 2_554
O1 Mn1 O2 91.91(3) 5_656 6_657
O1 Mn1 O2 88.09(3) . 6_657
O2 Mn1 O2 180.0 2_554 6_657
O1 Mn1 O3 89.84(3) 5_656 5_656
O1 Mn1 O3 90.16(3) . 5_656
O2 Mn1 O3 89.78(3) 2_554 5_656
O2 Mn1 O3 90.22(3) 6_657 5_656
O1 Mn1 O3 90.16(3) 5_656 .
O1 Mn1 O3 89.84(3) . .
O2 Mn1 O3 90.22(3) 2_554 .
O2 Mn1 O3 89.78(3) 6_657 .
O3 Mn1 O3 180.00(5) 5_656 .
C1 O1 Mn1 132.13(8) . .
C1 O2 Mn1 139.61(8) . 2
C2 O3 Mn1 134.95(10) . .
O2 C1 O1 127.05(11) . .
O2 C1 H1 116.5 . .
O1 C1 H1 116.5 . .
O3 C2 O3 129.84(19) . 8_565
O3 C2 H2A 104.8 . .
O3 C2 H2A 104.8 8_565 .
O3 C2 H2B 104.8 . .
O3 C2 H2B 104.8 8_565 .
H2A C2 H2B 105.8 . .
O3 C2 H2 115.1 . .
O3 C2 H2 115.1 8_565 .
H2A C2 H2 52.9 . .
H2B C2 H2 52.9 . .
C4 N7 C5 109.34(10) . .
C4 N7 C5 109.34(10) . 8_565
C5 N7 C5 110.04(15) . 8_565
C4 N7 C6 110.20(17) . .
C5 N7 C6 108.95(10) . .
C5 N7 C6 108.95(10) 8_565 .
N7 C4 H4A 109.4 . .
N7 C4 H4B 109.4 . .
H4A C4 H4B 109.5 . .
N7 C4 H4C 109.6 . .
H4A C4 H4C 105.5 . .
H4B C4 H4C 113.3 . .
N7 C5 H5A 109.5 . .
N7 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
N7 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N7 C6 H6A 109.5 . .
N7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.1987(8) 5_656
Mn1 O1 2.1988(8) .
Mn1 O2 2.2071(8) 2_554
Mn1 O2 2.2071(8) 6_657
Mn1 O3 2.2178(9) 5_656
Mn1 O3 2.2178(9) .
O1 C1 1.2418(14) .
O2 C1 1.2370(14) .
O2 Mn1 2.2071(8) 2
O3 C2 1.2257(13) .
C1 H1 0.9300 .
C2 O3 1.2258(13) 8_565
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C2 H2 0.9300 .
N7 C4 1.482(3) .
N7 C5 1.4838(15) .
N7 C5 1.4838(15) 8_565
N7 C6 1.492(2) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9570 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
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
O2 Mn1 O1 C1 -131.01(11) 2_554 .
O2 Mn1 O1 C1 48.99(11) 6_657 .
O3 Mn1 O1 C1 139.21(11) 5_656 .
O3 Mn1 O1 C1 -40.79(11) . .
O1 Mn1 O3 C2 47.18(14) 5_656 .
O1 Mn1 O3 C2 -132.82(14) . .
O2 Mn1 O3 C2 -40.91(14) 2_554 .
O2 Mn1 O3 C2 139.09(14) 6_657 .
Mn1 O2 C1 O1 -167.68(9) 2 .
Mn1 O1 C1 O2 176.07(9) . .
Mn1 O3 C2 O3 -177.37(9) . 8_565
