data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Ju-Hsiou Liao'
_publ_contact_author_email       CHEJHL@CCU.EDU.TW

_publ_section_title              
;
Synthesis, structure and hydrogen adsorption of a novel
porous metal-organic framework,
Mn9(btt)2(HCOO)12.0.7DMF.0.9H2O, where btt =
1,3,5-benzenetristetrazolate
;
loop_
_publ_author_name
'Ju-Hsiou Liao'
'Wan-Ting Chen'
'Cherng-Shiaw Tsai'
'Chih-Chieh Wang'
;
Ching-Chun Yang
;

data_MnBTT
_database_code_depnum_ccdc_archive 'CCDC 747863'
#=======================================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2.50 H1.50 Mn0.75 N2 O2'
_chemical_formula_weight         132.76

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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   11.7410(6)
_cell_length_b                   11.7410(6)
_cell_length_c                   13.3199(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1590.16(19)
_cell_formula_units_Z            12
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    916
_cell_measurement_theta_min      -23.529
_cell_measurement_theta_max      23.529

_exptl_crystal_description       'hexagonal rod'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             783
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.9038
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'phi-omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18794
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         28.26
_reflns_number_total             1372
_reflns_number_gt                1304
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER SMART'
_computing_cell_refinement       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep-3
_computing_publication_material  'wingx publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+4.0581P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1372
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.5000 0.5000 0.02216(18) Uani 1 2 d S . .
Mn2 Mn 0.3333 0.6667 0.39960(8) 0.0212(2) Uani 0.75 3 d SP . .
N1 N 0.5354(2) 0.5122(3) 0.66760(19) 0.0247(5) Uani 1 1 d . . .
N2 N 0.6047(3) 0.4566(3) 0.7018(2) 0.0288(6) Uani 1 1 d . . .
O1 O 0.2925(2) 0.3915(2) 0.5268(2) 0.0375(6) Uani 1 1 d . . .
O2 O 0.5021(2) 0.6872(2) 0.49332(19) 0.0302(5) Uani 1 1 d . . .
C1 C 0.4934(4) 0.5439(4) 0.7500 0.0197(8) Uani 1 2 d S . .
C2 C 0.4110(4) 0.6079(4) 0.7500 0.0201(8) Uani 1 2 d S . .
C3 C 0.2758(4) 0.5314(4) 0.7500 0.0221(8) Uani 1 2 d S . .
H3 H 0.2368 0.4403 0.7500 0.026 Uiso 1 2 calc SR . .
C4 C 0.1940(3) 0.4029(3) 0.5252(3) 0.0351(8) Uani 1 1 d . . .
H4 H 0.1174 0.3325 0.5507 0.042 Uiso 1 1 calc R . .

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 0.0261(3) 0.0216(3) 0.0227(3) 0.0002(2) -0.0018(3) 0.0149(3)
Mn2 0.0174(3) 0.0174(3) 0.0288(5) 0.000 0.000 0.00871(14)
N1 0.0262(12) 0.0338(13) 0.0226(13) 0.0010(11) 0.0003(10) 0.0214(11)
N2 0.0351(14) 0.0350(14) 0.0255(13) -0.0039(11) 0.0017(11) 0.0244(12)
O1 0.0255(11) 0.0380(13) 0.0562(16) 0.0066(12) 0.0028(11) 0.0212(10)
O2 0.0294(11) 0.0208(10) 0.0420(14) -0.0034(9) -0.0017(10) 0.0138(9)
C1 0.0144(17) 0.0207(18) 0.0236(19) 0.000 0.000 0.0085(15)
C2 0.0237(19) 0.0220(19) 0.0186(18) 0.000 0.000 0.0144(16)
C3 0.0235(19) 0.0180(18) 0.024(2) 0.000 0.000 0.0097(16)
C4 0.0242(15) 0.0347(17) 0.045(2) 0.0087(15) 0.0041(14) 0.0140(14)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.140(2) 7_666 ?
Mn1 O1 2.140(2) . ?
Mn1 O2 2.187(2) 7_666 ?
Mn1 O2 2.187(2) . ?
Mn1 N1 2.262(3) . ?
Mn1 N1 2.262(3) 7_666 ?
Mn2 O2 2.250(2) 2_665 ?
Mn2 O2 2.250(2) 3_565 ?
Mn2 O2 2.250(2) . ?
Mn2 N2 2.346(3) 9_556 ?
Mn2 N2 2.346(3) 8_566 ?
Mn2 N2 2.346(3) 7_666 ?
N1 C1 1.331(3) . ?
N1 N2 1.351(3) . ?
N2 N2 1.285(5) 10_557 ?
N2 Mn2 2.346(3) 7_666 ?
O1 C4 1.229(4) . ?
O2 C4 1.247(4) 2_665 ?
C1 N1 1.331(3) 10_557 ?
C1 C2 1.492(5) . ?
C2 C3 1.379(6) . ?
C2 C3 1.393(6) 2_665 ?
C3 C2 1.393(6) 3_565 ?
C4 O2 1.247(4) 3_565 ?

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
_geom_angle_publ_flag
O1 Mn1 O1 180.0 7_666 . ?
O1 Mn1 O2 92.43(9) 7_666 7_666 ?
O1 Mn1 O2 87.57(9) . 7_666 ?
O1 Mn1 O2 87.57(9) 7_666 . ?
O1 Mn1 O2 92.43(9) . . ?
O2 Mn1 O2 180.0 7_666 . ?
O1 Mn1 N1 90.50(10) 7_666 . ?
O1 Mn1 N1 89.50(10) . . ?
O2 Mn1 N1 86.16(9) 7_666 . ?
O2 Mn1 N1 93.84(9) . . ?
O1 Mn1 N1 89.50(10) 7_666 7_666 ?
O1 Mn1 N1 90.50(10) . 7_666 ?
O2 Mn1 N1 93.84(9) 7_666 7_666 ?
O2 Mn1 N1 86.16(9) . 7_666 ?
N1 Mn1 N1 180.0 . 7_666 ?
O2 Mn2 O2 92.20(9) 2_665 3_565 ?
O2 Mn2 O2 92.20(9) 2_665 . ?
O2 Mn2 O2 92.20(9) 3_565 . ?
O2 Mn2 N2 96.79(9) 2_665 9_556 ?
O2 Mn2 N2 81.78(9) 3_565 9_556 ?
O2 Mn2 N2 169.34(8) . 9_556 ?
O2 Mn2 N2 81.78(9) 2_665 8_566 ?
O2 Mn2 N2 169.34(8) 3_565 8_566 ?
O2 Mn2 N2 96.79(9) . 8_566 ?
N2 Mn2 N2 90.16(10) 9_556 8_566 ?
O2 Mn2 N2 169.34(9) 2_665 7_666 ?
O2 Mn2 N2 96.79(9) 3_565 7_666 ?
O2 Mn2 N2 81.78(9) . 7_666 ?
N2 Mn2 N2 90.16(10) 9_556 7_666 ?
N2 Mn2 N2 90.16(10) 8_566 7_666 ?
C1 N1 N2 104.7(2) . . ?
C1 N1 Mn1 138.6(2) . . ?
N2 N1 Mn1 115.95(18) . . ?
N2 N2 N1 109.69(15) 10_557 . ?
N2 N2 Mn2 125.15(7) 10_557 7_666 ?
N1 N2 Mn2 123.48(19) . 7_666 ?
C4 O1 Mn1 141.7(2) . . ?
C4 O2 Mn1 121.7(2) 2_665 . ?
C4 O2 Mn2 127.1(2) 2_665 . ?
Mn1 O2 Mn2 110.38(9) . . ?
N1 C1 N1 111.1(3) 10_557 . ?
N1 C1 C2 124.43(17) 10_557 . ?
N1 C1 C2 124.43(17) . . ?
C3 C2 C3 119.2(4) . 2_665 ?
C3 C2 C1 119.8(4) . . ?
C3 C2 C1 121.0(4) 2_665 . ?
C2 C3 C2 120.8(4) . 3_565 ?
O1 C4 O2 127.5(3) . 3_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.085