#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:19:04 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180332 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/01/7200185.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_7200185
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         '2(C6 H6 Co N27), 8(H2 O), O'
_chemical_formula_sum            'C12 H28 Co2 N54 O9'
_chemical_formula_weight         1190.74
_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                 102.104(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.3207(3)
_cell_length_b                   13.0862(4)
_cell_length_c                   15.3142(4)
_cell_measurement_reflns_used    5156
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.630
_cell_measurement_theta_min      1.84
_cell_volume                     2218.28(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  '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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33524
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADAB
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.143
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5156
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0619P)²+2.2570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                4345
_reflns_number_total             5071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809415b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7200185
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
Co1 Co 0.81885(3) 0.82690(2) 0.220920(19) 0.02271(12) Uani 1 1 d . . .
N19 N 0.92687(18) 0.75592(14) 0.16132(13) 0.0266(4) Uani 1 1 d . . .
N1 N 0.95501(17) 0.86355(15) 0.31264(13) 0.0262(4) Uani 1 1 d . . .
N6 N 0.71851(18) 0.89905(16) 0.28689(13) 0.0269(4) Uani 1 1 d . . .
N5 N 0.85938(19) 0.93402(18) 0.42403(14) 0.0311(5) Uani 1 1 d . . .
N24 N 0.84368(18) 0.94776(15) 0.15774(13) 0.0252(4) Uani 1 1 d . . .
N15 N 0.68767(19) 0.78777(16) 0.12542(14) 0.0295(4) Uani 1 1 d . . .
N10 N 0.78936(19) 0.70361(16) 0.28111(14) 0.0303(4) Uani 1 1 d . . .
N25 N 0.7816(2) 1.03622(16) 0.15796(15) 0.0344(5) Uani 1 1 d . . .
N7 N 0.5986(2) 0.91798(19) 0.25773(15) 0.0374(5) Uani 1 1 d . . .
N27 N 0.8982(2) 1.05303(17) 0.06270(15) 0.0358(5) Uani 1 1 d . . .
N26 N 0.8148(2) 1.09774(17) 0.10170(16) 0.0376(5) Uani 1 1 d . . .
N20 N 0.9654(2) 0.65761(17) 0.18098(18) 0.0426(6) Uani 1 1 d . . .
N23 N 0.9925(2) 0.89056(16) 0.07793(15) 0.0352(5) Uani 1 1 d . . .
H5 H 1.0404 0.9076 0.0436 0.042 Uiso 1 1 calc R . .
N22 N 1.0732(2) 0.72324(17) 0.09755(16) 0.0369(5) Uani 1 1 d . . .
H6 H 1.1274 0.7295 0.0660 0.044 Uiso 1 1 calc R . .
N11 N 0.8409(3) 0.6810(2) 0.36784(17) 0.0456(6) Uani 1 1 d . . .
N4 N 1.07138(19) 0.92754(18) 0.43253(14) 0.0339(5) Uani 1 1 d . . .
N2 N 1.07191(19) 0.85442(18) 0.30464(15) 0.0345(5) Uani 1 1 d . . .
N9 N 0.6513(2) 0.97855(18) 0.38898(15) 0.0360(5) Uani 1 1 d . . .
H2 H 0.6476 1.0085 0.4383 0.043 Uiso 1 1 calc R . .
N3 N 1.1392(2) 0.89237(19) 0.37639(15) 0.0374(5) Uani 1 1 d . . .
N18 N 0.5682(2) 0.6927(2) 0.02672(19) 0.0496(7) Uani 1 1 d . . .
N8 N 0.5585(2) 0.9660(2) 0.31880(17) 0.0430(6) Uani 1 1 d . . .
N17 N 0.5728(3) 0.7882(2) -0.00566(18) 0.0520(7) Uani 1 1 d . . .
N21 N 1.0524(3) 0.63843(18) 0.14244(19) 0.0487(6) Uani 1 1 d . . .
N12 N 0.8115(3) 0.5892(2) 0.3844(2) 0.0581(8) Uani 1 1 d . . .
N13 N 0.7410(3) 0.5511(2) 0.3089(2) 0.0594(8) Uani 1 1 d . . .
H4 H 0.7106 0.4906 0.3027 0.071 Uiso 1 1 calc R . .
N14 N 0.6622(3) 0.6138(2) 0.1622(2) 0.0546(8) Uani 1 1 d . . .
N16 N 0.6436(2) 0.8454(2) 0.05174(17) 0.0447(6) Uani 1 1 d . . .
C2 C 0.7494(2) 0.93700(18) 0.36928(15) 0.0270(5) Uani 1 1 d . . .
C3 C 0.6394(2) 0.6959(2) 0.1066(2) 0.0375(6) Uani 1 1 d . . .
C1 C 0.9586(2) 0.90885(18) 0.39091(15) 0.0269(5) Uani 1 1 d . . .
C4 C 0.7265(3) 0.6221(2) 0.2465(2) 0.0409(6) Uani 1 1 d . . .
C6 C 0.9137(2) 0.96108(18) 0.09891(16) 0.0279(5) Uani 1 1 d . . .
C5 C 0.9961(2) 0.79495(19) 0.11031(15) 0.0276(5) Uani 1 1 d . . .
O1 O 0.61883(19) 0.05862(15) 0.54291(13) 0.0320(4) Uani 1 1 d . . .
O2 O 0.2667(2) 0.75043(19) 0.0290(2) 0.0493(6) Uani 1 1 d . . .
O3 O 0.4247(6) 0.8144(4) 0.8117(3) 0.1340(18) Uani 1 1 d D . .
O4 O 0.6804(8) 0.3537(5) 0.2916(7) 0.292(6) Uani 1 1 d D . .
O5 O 0.5921(5) 0.4525(5) 0.4261(4) 0.0828(18) Uani 0.50 1 d P . .
H1 H 0.870(3) 0.971(3) 0.465(2) 0.052(10) Uiso 1 1 d . . .
H3 H 0.633(4) 0.568(4) 0.150(3) 0.072(14) Uiso 1 1 d . . .
H7 H 0.302(4) 0.787(4) 0.063(3) 0.069(15) Uiso 1 1 d . . .
H8 H 0.246(4) 0.779(4) -0.013(3) 0.070(16) Uiso 1 1 d . . .
H10 H 0.459(4) 0.869(2) 0.840(3) 0.069(14) Uiso 1 1 d D . .
H9 H 0.352(5) 0.828(18) 0.81(3) 1.0(3) Uiso 1 1 d D . .
H12 H 0.678(3) 0.303(2) 0.258(2) 0.042(10) Uiso 1 1 d D . .
H13 H 0.676(4) 0.091(3) 0.560(2) 0.050(11) Uiso 1 1 d . . .
H14 H 0.564(3) 0.098(3) 0.523(2) 0.052(10) Uiso 1 1 d . . .
H11 H 0.622(2) 0.346(2) 0.3174(19) 0.021(7) Uiso 1 1 d 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'
Co Co 0.3494 0.9721 '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
N24 Co1 N19 89.06(8) . . ?
N24 Co1 N1 89.01(8) . . ?
N19 Co1 N1 88.56(8) . . ?
N24 Co1 N6 91.46(8) . . ?
N19 Co1 N6 176.50(8) . . ?
N1 Co1 N6 87.99(8) . . ?
N24 Co1 N10 177.96(9) . . ?
N19 Co1 N10 90.80(9) . . ?
N1 Co1 N10 93.01(9) . . ?
N6 Co1 N10 88.80(9) . . ?
N24 Co1 N15 90.43(9) . . ?
N19 Co1 N15 88.67(9) . . ?
N1 Co1 N15 177.18(8) . . ?
N6 Co1 N15 94.79(9) . . ?
N10 Co1 N15 87.54(9) . . ?
C5 N19 N20 107.0(2) . . ?
C5 N19 Co1 127.80(17) . . ?
N20 N19 Co1 123.82(16) . . ?
C1 N1 N2 105.88(19) . . ?
C1 N1 Co1 129.81(17) . . ?
N2 N1 Co1 124.10(15) . . ?
C2 N6 N7 106.8(2) . . ?
C2 N6 Co1 127.95(17) . . ?
N7 N6 Co1 125.24(16) . . ?
C2 N5 C1 120.0(2) . . ?
C2 N5 H1 117(3) . . ?
C1 N5 H1 116(3) . . ?
C6 N24 N25 105.83(19) . . ?
C6 N24 Co1 128.67(16) . . ?
N25 N24 Co1 125.20(15) . . ?
C3 N15 N16 105.0(2) . . ?
C3 N15 Co1 128.61(19) . . ?
N16 N15 Co1 124.96(17) . . ?
C4 N10 N11 107.3(2) . . ?
C4 N10 Co1 127.91(19) . . ?
N11 N10 Co1 124.49(18) . . ?
N26 N25 N24 107.92(19) . . ?
N8 N7 N6 109.3(2) . . ?
C6 N27 N26 104.6(2) . . ?
N25 N26 N27 110.7(2) . . ?
N21 N20 N19 108.9(2) . . ?
C5 N23 C6 120.8(2) . . ?
C5 N23 H5 119.6 . . ?
C6 N23 H5 119.6 . . ?
C5 N22 N21 108.4(2) . . ?
C5 N22 H6 125.8 . . ?
N21 N22 H6 125.8 . . ?
N12 N11 N10 108.6(2) . . ?
C1 N4 N3 104.51(19) . . ?
N3 N2 N1 107.5(2) . . ?
C2 N9 N8 108.6(2) . . ?
C2 N9 H2 125.7 . . ?
N8 N9 H2 125.7 . . ?
N2 N3 N4 111.0(2) . . ?
C3 N18 N17 104.4(2) . . ?
N7 N8 N9 107.8(2) . . ?
N16 N17 N18 110.6(2) . . ?
N20 N21 N22 107.9(2) . . ?
N11 N12 N13 107.8(2) . . ?
C4 N13 N12 108.7(3) . . ?
C4 N13 H4 125.6 . . ?
N12 N13 H4 125.6 . . ?
C4 N14 C3 121.9(3) . . ?
C4 N14 H3 118(4) . . ?
C3 N14 H3 119(4) . . ?
N17 N16 N15 108.0(2) . . ?
N9 C2 N6 107.6(2) . . ?
N9 C2 N5 125.3(2) . . ?
N6 C2 N5 127.1(2) . . ?
N18 C3 N15 112.0(3) . . ?
N18 C3 N14 123.6(3) . . ?
N15 C3 N14 124.3(3) . . ?
N4 C1 N1 111.1(2) . . ?
N4 C1 N5 124.1(2) . . ?
N1 C1 N5 124.7(2) . . ?
N13 C4 N10 107.5(3) . . ?
N13 C4 N14 126.7(3) . . ?
N10 C4 N14 125.7(3) . . ?
N27 C6 N24 111.0(2) . . ?
N27 C6 N23 123.5(2) . . ?
N24 C6 N23 125.5(2) . . ?
N19 C5 N22 107.8(2) . . ?
N19 C5 N23 127.1(2) . . ?
N22 C5 N23 125.1(2) . . ?
H13 O1 H14 107(4) . . ?
H7 O2 H8 107(5) . . ?
H10 O3 H9 98(2) . . ?
H12 O4 H11 106(2) . . ?
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
Co1 N24 1.906(2) . ?
Co1 N19 1.9128(19) . ?
Co1 N1 1.916(2) . ?
Co1 N6 1.919(2) . ?
Co1 N10 1.922(2) . ?
Co1 N15 1.922(2) . ?
N19 C5 1.320(3) . ?
N19 N20 1.372(3) . ?
N1 C1 1.330(3) . ?
N1 N2 1.360(3) . ?
N6 C2 1.333(3) . ?
N6 N7 1.360(3) . ?
N5 C2 1.348(3) . ?
N5 C1 1.367(3) . ?
N5 H1 0.78(4) . ?
N24 C6 1.331(3) . ?
N24 N25 1.354(3) . ?
N15 C3 1.326(3) . ?
N15 N16 1.362(3) . ?
N10 C4 1.329(3) . ?
N10 N11 1.366(3) . ?
N25 N26 1.291(3) . ?
N7 N8 1.285(3) . ?
N27 C6 1.321(3) . ?
N27 N26 1.351(3) . ?
N20 N21 1.274(3) . ?
N23 C5 1.343(3) . ?
N23 C6 1.368(3) . ?
N23 H5 0.8600 . ?
N22 C5 1.324(3) . ?
N22 N21 1.352(3) . ?
N22 H6 0.8600 . ?
N11 N12 1.286(4) . ?
N4 C1 1.324(3) . ?
N4 N3 1.348(3) . ?
N2 N3 1.298(3) . ?
N9 C2 1.327(3) . ?
N9 N8 1.346(3) . ?
N9 H2 0.8600 . ?
N18 C3 1.317(4) . ?
N18 N17 1.349(4) . ?
N17 N16 1.296(3) . ?
N12 N13 1.355(4) . ?
N13 C4 1.318(4) . ?
N13 H4 0.8600 . ?
N14 C4 1.346(4) . ?
N14 C3 1.363(4) . ?
N14 H3 0.69(5) . ?
O1 H13 0.77(4) . ?
O1 H14 0.81(4) . ?
O2 H7 0.76(5) . ?
O2 H8 0.74(5) . ?
O3 H10 0.881(10) . ?
O3 H9 0.849(11) . ?
O4 H12 0.840(10) . ?
O4 H11 0.846(10) . ?
