#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003988.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_7003988
loop_
_publ_author_name
'Briceño, Alexander'
'Fulgence, Aaron'
'Hill, Yennifer'
'Atencio, Reinaldo'
_publ_section_title
;
 A non-photochemical route for the regioselective preparation of
 rtct-pyridylcyclobutanes via hydrothermal isomerisation promoted by
 polymolybdates
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              3275
_journal_page_last               3278
_journal_paper_doi               10.1039/b801845f
_journal_year                    2008
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C24 H24 N4, Mo8 O26'
_chemical_formula_sum            'C24 H24 Mo8 N4 O26'
_chemical_formula_weight         1551.99
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.800(4)
_cell_angle_beta                 108.104(6)
_cell_angle_gamma                99.049(5)
_cell_formula_units_Z            1
_cell_length_a                   9.704(2)
_cell_length_b                   10.070(2)
_cell_length_c                   10.482(2)
_cell_measurement_reflns_used    1850
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.02
_cell_volume                     939.0(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics
;
SHELXLTL-NT V5.1 (Bruker AXS, 1998) and DIAMOND
(Brandenburg, 1998)
;
_computing_publication_material
;
SHELXLTL-NT V5.1 (Bruker AXS, 1998) and PLATON (Spek, 2003).
;
_computing_structure_refinement  'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_computing_structure_solution    'SHELXLTL-NT V5.1 (Bruker AXS, 1998)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.778
_diffrn_measurement_device
;
Mercury (2x2 bin mode)
;
_diffrn_measurement_device_type  'Rigaku AFC7S Mercury'
_diffrn_measurement_method       'ω '
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10775
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.685
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0376P)²+2.1503P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                2992
_reflns_number_total             3551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801845f.txt
_cod_data_source_block           shelxle1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        939.0(4)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003988
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Mo1 Mo 0.70441(5) -0.23558(4) 0.66008(4) 0.02167(13) Uani 1 1 d . . .
Mo2 Mo 0.31392(4) -0.03827(4) 0.50380(4) 0.01628(12) Uani 1 1 d . . .
Mo3 Mo 0.56395(5) 0.28742(4) 0.63265(4) 0.01888(13) Uani 1 1 d . . .
Mo4 Mo 0.58252(4) 0.01386(4) 0.78893(4) 0.01797(13) Uani 1 1 d . . .
O1 O 0.4298(3) 0.0967(3) 0.6736(3) 0.0177(7) Uani 1 1 d . . .
O2 O 0.4693(4) -0.0986(4) 0.8368(4) 0.0249(8) Uani 1 1 d . . .
O3 O 0.1956(4) 0.0638(4) 0.4299(3) 0.0233(8) Uani 1 1 d . . .
O4 O 0.3741(4) 0.3136(3) 0.5344(4) 0.0235(8) Uani 1 1 d . . .
O5 O 0.5196(3) -0.1087(3) 0.5678(3) 0.0187(7) Uani 1 1 d . . .
O6 O 0.7463(4) -0.0713(4) 0.8000(3) 0.0237(8) Uani 1 1 d . . .
O7 O 0.6963(3) 0.1530(3) 0.6685(3) 0.0189(7) Uani 1 1 d . . .
O8 O 0.6743(4) 0.3923(4) 0.5737(4) 0.0282(9) Uani 1 1 d . . .
O9 O 0.2097(4) -0.1490(4) 0.5596(4) 0.0249(8) Uani 1 1 d . . .
O10 O 0.6674(4) 0.1453(4) 0.9295(4) 0.0329(9) Uani 1 1 d . . .
O11 O 0.5887(4) -0.3401(4) 0.7126(4) 0.0320(9) Uani 1 1 d . . .
O12 O 0.5959(4) 0.3704(4) 0.7964(4) 0.0301(9) Uani 1 1 d . . .
O13 O 0.8698(4) -0.2848(4) 0.7095(4) 0.0366(10) Uani 1 1 d . . .
N1 N 0.0110(5) 0.1589(5) -0.1105(5) 0.0357(12) Uani 1 1 d . . .
H1N H -0.0833 0.1328 -0.1300 0.043 Uiso 1 1 calc R . .
N2 N -0.2072(5) 0.5052(5) 0.3861(5) 0.0369(12) Uani 1 1 d . . .
H2N H -0.2540 0.5109 0.4435 0.044 Uiso 1 1 calc R . .
C1 C -0.0268(6) 0.3849(5) -0.0283(5) 0.0266(12) Uani 1 1 d . . .
H1 H -0.1272 0.3320 -0.0463 0.032 Uiso 1 1 calc R . .
C2 C 0.0298(6) 0.4920(6) 0.1081(5) 0.0282(12) Uani 1 1 d . . .
H2 H 0.1328 0.4905 0.1592 0.034 Uiso 1 1 calc R . .
C3 C 0.0772(6) 0.2913(6) -0.0467(5) 0.0266(12) Uani 1 1 d . . .
C4 C 0.0859(7) 0.0671(6) -0.1443(6) 0.0384(14) Uani 1 1 d . . .
H4 H 0.0351 -0.0228 -0.1881 0.046 Uiso 1 1 calc R . .
C5 C 0.2347(6) 0.1024(6) -0.1161(6) 0.0343(14) Uani 1 1 d . . .
H5 H 0.2859 0.0385 -0.1418 0.041 Uiso 1 1 calc R . .
C6 C 0.3080(6) 0.2349(6) -0.0487(6) 0.0340(13) Uani 1 1 d . . .
H6 H 0.4102 0.2612 -0.0272 0.041 Uiso 1 1 calc R . .
C7 C 0.2293(7) 0.3299(6) -0.0125(6) 0.0308(13) Uani 1 1 d . . .
H7 H 0.2791 0.4192 0.0346 0.037 Uiso 1 1 calc R . .
C8 C -0.0604(6) 0.4907(6) 0.2033(5) 0.0274(12) Uani 1 1 d . . .
C9 C -0.1789(7) 0.3862(6) 0.1896(5) 0.0321(13) Uani 1 1 d . . .
H9 H -0.2094 0.3102 0.1168 0.039 Uiso 1 1 calc R . .
C10 C -0.2516(6) 0.3943(6) 0.2829(6) 0.0339(13) Uani 1 1 d . . .
H10 H -0.3304 0.3239 0.2746 0.041 Uiso 1 1 calc R . .
C11 C -0.0931(7) 0.6071(6) 0.4031(6) 0.0345(14) Uani 1 1 d . . .
H11 H -0.0644 0.6822 0.4765 0.041 Uiso 1 1 calc R . .
C12 C -0.0195(6) 0.6006(5) 0.3134(6) 0.0287(12) Uani 1 1 d . . .
H12 H 0.0604 0.6716 0.3259 0.034 Uiso 1 1 calc R . .
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'
Mo Mo -1.6832 0.6857 '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'
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
O11 Mo1 O13 105.84(19) . . ?
O11 Mo1 O4 99.68(17) . 2_656 ?
O13 Mo1 O4 102.38(17) . 2_656 ?
O11 Mo1 O6 98.66(17) . . ?
O13 Mo1 O6 100.71(18) . . ?
O4 Mo1 O6 145.17(15) 2_656 . ?
O11 Mo1 O3 163.48(16) . 2_656 ?
O13 Mo1 O3 90.64(16) . 2_656 ?
O4 Mo1 O3 77.45(14) 2_656 2_656 ?
O6 Mo1 O3 76.58(14) . 2_656 ?
O11 Mo1 O5 93.21(15) . . ?
O13 Mo1 O5 160.90(16) . . ?
O4 Mo1 O5 75.21(13) 2_656 . ?
O6 Mo1 O5 74.43(13) . . ?
O3 Mo1 O5 70.30(12) 2_656 . ?
O9 Mo2 O3 104.51(17) . . ?
O9 Mo2 O1 101.62(15) . . ?
O3 Mo2 O1 97.13(15) . . ?
O9 Mo2 O7 100.94(16) . 2_656 ?
O3 Mo2 O7 96.56(15) . 2_656 ?
O1 Mo2 O7 149.66(14) . 2_656 ?
O9 Mo2 O5 99.06(16) . . ?
O3 Mo2 O5 156.42(15) . . ?
O1 Mo2 O5 77.89(13) . . ?
O7 Mo2 O5 78.76(13) 2_656 . ?
O9 Mo2 O5 174.72(15) . 2_656 ?
O3 Mo2 O5 80.76(14) . 2_656 ?
O1 Mo2 O5 77.52(12) . 2_656 ?
O7 Mo2 O5 78.14(12) 2_656 2_656 ?
O5 Mo2 O5 75.66(14) . 2_656 ?
O9 Mo2 Mo4 90.05(12) . . ?
O3 Mo2 Mo4 133.05(11) . . ?
O1 Mo2 Mo4 35.92(10) . . ?
O7 Mo2 Mo4 124.59(10) 2_656 . ?
O5 Mo2 Mo4 45.84(8) . . ?
O5 Mo2 Mo4 86.28(8) 2_656 . ?
O12 Mo3 O8 105.00(18) . . ?
O12 Mo3 O4 103.40(17) . . ?
O8 Mo3 O4 101.03(17) . . ?
O12 Mo3 O7 100.22(16) . . ?
O8 Mo3 O7 95.67(16) . . ?
O4 Mo3 O7 146.27(14) . . ?
O12 Mo3 O1 88.58(15) . . ?
O8 Mo3 O1 163.75(15) . . ?
O4 Mo3 O1 84.03(14) . . ?
O7 Mo3 O1 72.77(12) . . ?
O12 Mo3 O5 159.94(15) . 2_656 ?
O8 Mo3 O5 94.55(15) . 2_656 ?
O4 Mo3 O5 76.67(13) . 2_656 ?
O7 Mo3 O5 72.94(12) . 2_656 ?
O1 Mo3 O5 71.41(11) . 2_656 ?
O2 Mo4 O10 105.30(18) . . ?
O2 Mo4 O6 102.64(16) . . ?
O10 Mo4 O6 98.21(17) . . ?
O2 Mo4 O1 98.51(16) . . ?
O10 Mo4 O1 101.09(16) . . ?
O6 Mo4 O1 146.34(14) . . ?
O2 Mo4 O5 96.18(15) . . ?
O10 Mo4 O5 158.49(16) . . ?
O6 Mo4 O5 77.70(13) . . ?
O1 Mo4 O5 74.22(12) . . ?
O2 Mo4 O7 166.16(14) . . ?
O10 Mo4 O7 86.47(15) . . ?
O6 Mo4 O7 82.41(14) . . ?
O1 Mo4 O7 71.61(12) . . ?
O5 Mo4 O7 72.09(11) . . ?
O2 Mo4 Mo2 86.68(12) . . ?
O10 Mo4 Mo2 136.37(13) . . ?
O6 Mo4 Mo2 120.29(10) . . ?
O1 Mo4 Mo2 35.29(9) . . ?
O5 Mo4 Mo2 42.58(8) . . ?
O7 Mo4 Mo2 79.69(8) . . ?
Mo2 O1 Mo4 108.79(15) . . ?
Mo2 O1 Mo3 111.88(14) . . ?
Mo4 O1 Mo3 104.74(13) . . ?
Mo2 O3 Mo1 116.48(16) . 2_656 ?
Mo3 O4 Mo1 116.90(17) . 2_656 ?
Mo2 O5 Mo4 91.58(12) . . ?
Mo2 O5 Mo3 91.70(11) . 2_656 ?
Mo4 O5 Mo3 163.86(16) . 2_656 ?
Mo2 O5 Mo2 104.34(14) . 2_656 ?
Mo4 O5 Mo2 98.23(12) . 2_656 ?
Mo3 O5 Mo2 96.25(12) 2_656 2_656 ?
Mo2 O5 Mo1 163.19(17) . . ?
Mo4 O5 Mo1 86.58(11) . . ?
Mo3 O5 Mo1 85.72(11) 2_656 . ?
Mo2 O5 Mo1 92.45(11) 2_656 . ?
Mo4 O6 Mo1 114.74(16) . . ?
Mo2 O7 Mo3 110.85(15) 2_656 . ?
Mo2 O7 Mo4 108.99(14) 2_656 . ?
Mo3 O7 Mo4 101.64(14) . . ?
C4 N1 C3 122.7(5) . . ?
C4 N1 H1N 118.6 . . ?
C3 N1 H1N 118.6 . . ?
C11 N2 C10 122.4(5) . . ?
C11 N2 H2N 118.8 . . ?
C10 N2 H2N 118.8 . . ?
C3 C1 C2 115.5(4) . . ?
C3 C1 C2 115.9(4) . 2_565 ?
C2 C1 C2 89.0(4) . 2_565 ?
C3 C1 H1 111.6 . . ?
C2 C1 H1 111.6 . . ?
C2 C1 H1 111.6 2_565 . ?
C8 C2 C1 119.2(4) . . ?
C8 C2 C1 116.1(4) . 2_565 ?
C1 C2 C1 91.0(4) . 2_565 ?
C8 C2 H2 109.7 . . ?
C1 C2 H2 109.7 . . ?
C1 C2 H2 109.7 2_565 . ?
N1 C3 C7 117.6(5) . . ?
N1 C3 C1 115.6(5) . . ?
C7 C3 C1 126.6(5) . . ?
N1 C4 C5 121.2(6) . . ?
N1 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 118.4(5) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C7 120.0(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C3 C7 C6 119.9(5) . . ?
C3 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C12 C8 C9 117.4(5) . . ?
C12 C8 C2 117.5(5) . . ?
C9 C8 C2 125.0(5) . . ?
C10 C9 C8 120.3(5) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
N2 C10 C9 119.0(5) . . ?
N2 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
N2 C11 C12 119.6(5) . . ?
N2 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C8 121.3(5) . . ?
C11 C12 H12 119.3 . . ?
C8 C12 H12 119.3 . . ?
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
Mo1 O11 1.691(4) . ?
Mo1 O13 1.704(4) . ?
Mo1 O4 1.926(3) 2_656 ?
Mo1 O6 1.931(4) . ?
Mo1 O3 2.316(4) 2_656 ?
Mo1 O5 2.409(3) . ?
Mo2 O9 1.680(3) . ?
Mo2 O3 1.743(3) . ?
Mo2 O1 1.953(3) . ?
Mo2 O7 1.954(3) 2_656 ?
Mo2 O5 2.167(3) . ?
Mo2 O5 2.388(3) 2_656 ?
Mo2 Mo4 3.2015(8) . ?
Mo3 O12 1.700(4) . ?
Mo3 O8 1.702(4) . ?
Mo3 O4 1.892(3) . ?
Mo3 O7 2.006(3) . ?
Mo3 O1 2.319(3) . ?
Mo3 O5 2.374(3) 2_656 ?
Mo4 O2 1.693(4) . ?
Mo4 O10 1.705(4) . ?
Mo4 O6 1.902(4) . ?
Mo4 O1 1.984(3) . ?
Mo4 O5 2.297(3) . ?
Mo4 O7 2.387(3) . ?
O3 Mo1 2.316(4) 2_656 ?
O4 Mo1 1.926(3) 2_656 ?
O5 Mo3 2.374(3) 2_656 ?
O5 Mo2 2.388(3) 2_656 ?
O7 Mo2 1.954(3) 2_656 ?
N1 C4 1.334(7) . ?
N1 C3 1.352(7) . ?
N1 H1N 0.8600 . ?
N2 C11 1.332(7) . ?
N2 C10 1.339(7) . ?
N2 H2N 0.8600 . ?
C1 C3 1.520(7) . ?
C1 C2 1.538(7) . ?
C1 C2 1.597(7) 2_565 ?
C1 H1 0.9800 . ?
C2 C8 1.518(8) . ?
C2 C1 1.597(7) 2_565 ?
C2 H2 0.9800 . ?
C3 C7 1.380(8) . ?
C4 C5 1.357(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(8) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C12 1.378(7) . ?
C8 C9 1.386(8) . ?
C9 C10 1.372(8) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.345(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
