#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:19:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180332 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/01/7200187.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_7200187
loop_
_publ_author_name
'Lin, Jiao-Min'
'Huang, Bei-Shu'
'Guan, Yang-Fan'
'Liu, Zhao-Qing'
'Wang, Dong-Yao'
'Dong, Wen'
_publ_section_title
;
 Syntheses, structures and properties of seven H2BTA coordinating 3-D
 metallic complexes containing 0-, 1-, 2-, and 3-D frameworks (H2BTA =
 bis(tetrazolyl)amine)
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              329
_journal_paper_doi               10.1039/b809415b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C4 H6 Mn N18 Na2 O2'
_chemical_formula_sum            'C4 H6 Mn N18 Na2 O2'
_chemical_formula_weight         439.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4412(2)
_cell_length_b                   9.6151(2)
_cell_length_c                   8.6398(2)
_cell_measurement_reflns_used    1714
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.510
_cell_measurement_theta_min      2.28
_cell_volume                     742.13(3)
_computing_cell_refinement       'SAINT (Bruker, 2001-2005)'
_computing_data_collection       'SMART (Bruker, 2001-2005) '
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001-2005)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6008
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.022(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   1.057
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0317P)²+0.3461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                1396
_reflns_number_total             1614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809415b.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7200187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.5000 0.0000 0.01558(15) Uani 1 2 d S . .
Na1 Na 0.38706(10) 0.30763(10) 0.05534(12) 0.0323(3) Uani 1 1 d . . .
N2 N 0.35178(19) 0.5638(2) 0.0810(2) 0.0253(4) Uani 1 1 d . . .
N1 N 0.22542(18) 0.59707(18) 0.1165(2) 0.0217(4) Uani 1 1 d . . .
N3 N 0.4417(2) 0.6692(2) 0.1144(3) 0.0334(5) Uani 1 1 d . . .
N4 N 0.3810(2) 0.7754(2) 0.1753(3) 0.0355(5) Uani 1 1 d . . .
C1 C 0.2495(2) 0.7257(2) 0.1741(3) 0.0212(5) Uani 1 1 d . . .
N7 N -0.1699(2) 0.6305(2) 0.2340(2) 0.0255(4) Uani 1 1 d . . .
N9 N -0.05238(19) 0.82137(19) 0.3291(2) 0.0228(4) Uani 1 1 d . . .
N8 N -0.17315(19) 0.7413(2) 0.3189(2) 0.0252(4) Uani 1 1 d . . .
C2 C 0.0210(2) 0.7532(2) 0.2452(3) 0.0193(5) Uani 1 1 d . . .
N6 N -0.04705(19) 0.63542(19) 0.1840(2) 0.0212(4) Uani 1 1 d . . .
N5 N 0.1505(2) 0.8033(2) 0.2253(3) 0.0311(5) Uani 1 1 d . . .
O2 O 0.3575(3) 0.0680(3) -0.0034(4) 0.0663(7) Uani 1 1 d . . .
H1 H 0.179(3) 0.882(3) 0.261(3) 0.042(8) Uiso 1 1 d . . .
H3 H 0.353(6) 0.028(6) 0.063(7) 0.11(2) Uiso 1 1 d . . .
H2 H 0.358(16) 0.036(15) -0.06(2) 0.49(11) Uiso 1 1 d . . .
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'
Na Na 0.0362 0.0249 '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
_geom_angle_publ_flag
N1 Mn1 N1 180.0 . 3_565 ?
N1 Mn1 N6 79.29(6) . . ?
N1 Mn1 N6 100.71(6) 3_565 . ?
N1 Mn1 N6 100.71(6) . 3_565 ?
N1 Mn1 N6 79.29(6) 3_565 3_565 ?
N6 Mn1 N6 180.00(6) . 3_565 ?
N1 Mn1 N9 87.21(7) . 4_575 ?
N1 Mn1 N9 92.79(7) 3_565 4_575 ?
N6 Mn1 N9 88.24(7) . 4_575 ?
N6 Mn1 N9 91.76(7) 3_565 4_575 ?
N1 Mn1 N9 92.79(7) . 2_545 ?
N1 Mn1 N9 87.21(7) 3_565 2_545 ?
N6 Mn1 N9 91.76(7) . 2_545 ?
N6 Mn1 N9 88.24(7) 3_565 2_545 ?
N9 Mn1 N9 180.00(6) 4_575 2_545 ?
O2 Na1 N2 166.09(10) . . ?
O2 Na1 N3 90.83(10) . 3_665 ?
N2 Na1 N3 95.35(7) . 3_665 ?
O2 Na1 N8 78.52(9) . 2_545 ?
N2 Na1 N8 93.41(7) . 2_545 ?
N3 Na1 N8 166.70(7) 3_665 2_545 ?
O2 Na1 N4 94.67(10) . 2_645 ?
N2 Na1 N4 97.66(7) . 2_645 ?
N3 Na1 N4 91.02(7) 3_665 2_645 ?
N8 Na1 N4 97.72(7) 2_545 2_645 ?
O2 Na1 N7 90.82(10) . 3_565 ?
N2 Na1 N7 77.60(6) . 3_565 ?
N3 Na1 N7 83.18(7) 3_665 3_565 ?
N8 Na1 N7 88.96(6) 2_545 3_565 ?
N4 Na1 N7 172.08(7) 2_645 3_565 ?
N3 N2 N1 108.95(17) . . ?
N3 N2 Na1 133.94(14) . . ?
N1 N2 Na1 113.71(13) . . ?
C1 N1 N2 104.32(16) . . ?
C1 N1 Mn1 125.44(14) . . ?
N2 N1 Mn1 125.02(13) . . ?
N2 N3 N4 110.30(18) . . ?
N2 N3 Na1 115.97(15) . 3_665 ?
N4 N3 Na1 126.18(15) . 3_665 ?
C1 N4 N3 103.73(18) . . ?
C1 N4 Na1 123.72(16) . 2_655 ?
N3 N4 Na1 95.52(14) . 2_655 ?
N4 C1 N1 112.70(19) . . ?
N4 C1 N5 122.2(2) . . ?
N1 C1 N5 125.07(19) . . ?
N8 N7 N6 109.16(16) . . ?
N8 N7 Na1 100.96(13) . 3_565 ?
N6 N7 Na1 99.54(12) . 3_565 ?
C2 N9 N8 105.13(17) . . ?
C2 N9 Mn1 134.77(14) . 2 ?
N8 N9 Mn1 119.06(13) . 2 ?
N7 N8 N9 109.24(17) . . ?
N7 N8 Na1 125.90(13) . 2 ?
N9 N8 Na1 124.82(13) . 2 ?
N6 C2 N9 111.64(18) . . ?
N6 C2 N5 125.87(19) . . ?
N9 C2 N5 122.48(19) . . ?
C2 N6 N7 104.83(16) . . ?
C2 N6 Mn1 127.35(14) . . ?
N7 N6 Mn1 126.69(13) . . ?
C2 N5 C1 125.0(2) . . ?
C2 N5 H1 118.1(19) . . ?
C1 N5 H1 116.1(19) . . ?
Na1 O2 H3 113(5) . . ?
Na1 O2 H2 130(10) . . ?
H3 O2 H2 117(10) . . ?
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 N1 2.2423(17) . ?
Mn1 N1 2.2423(17) 3_565 ?
Mn1 N6 2.2083(17) . ?
Mn1 N6 2.2083(17) 3_565 ?
Mn1 N9 2.2143(17) 4_575 ?
Mn1 N9 2.2143(17) 2_545 ?
Na1 O2 2.357(3) . ?
Na1 N2 2.505(2) . ?
Na1 N3 2.519(2) 3_665 ?
Na1 N8 2.662(2) 2_545 ?
Na1 N4 2.647(2) 2_645 ?
Na1 N7 2.737(2) 3_565 ?
N2 N3 1.294(3) . ?
N2 N1 1.363(2) . ?
N1 C1 1.325(3) . ?
N3 N4 1.358(3) . ?
N3 Na1 2.519(2) 3_665 ?
N4 C1 1.327(3) . ?
N4 Na1 2.647(2) 2_655 ?
C1 N5 1.377(3) . ?
N7 N8 1.299(3) . ?
N7 N6 1.363(2) . ?
N7 Na1 2.737(2) 3_565 ?
N9 C2 1.327(3) . ?
N9 N8 1.355(2) . ?
N9 Mn1 2.2143(17) 2 ?
N8 Na1 2.662(2) 2 ?
C2 N6 1.325(3) . ?
C2 N5 1.375(3) . ?
N5 H1 0.83(3) . ?
O2 H3 0.70(6) . ?
O2 H2 0.61(15) . ?
