#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003987.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_7003987
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                100.807(5)
_cell_angle_beta                 106.923(4)
_cell_angle_gamma                97.085(5)
_cell_formula_units_Z            1
_cell_length_a                   9.620(2)
_cell_length_b                   10.087(2)
_cell_length_c                   10.578(3)
_cell_measurement_reflns_used    2490
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.14
_cell_volume                     947.1(4)
_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 0.974
_diffrn_measured_fraction_theta_max 0.765
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10969
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    2.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.956
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0477
_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)+(0.0564P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                2746
_reflns_number_total             3580
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801845f.txt
_cod_data_source_block           shelxle2
_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        947.2(4)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003987
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 0.56380(6) 0.28990(5) 1.13105(5) 0.02086(18) Uani 1 1 d . . .
Mo2 Mo 0.68905(5) 0.02856(5) 1.00195(5) 0.01729(17) Uani 1 1 d . . .
Mo3 Mo 0.30967(6) 0.24137(5) 0.83736(6) 0.02356(18) Uani 1 1 d . . .
Mo4 Mo 0.43164(6) -0.02246(5) 0.71488(5) 0.01965(17) Uani 1 1 d . . .
O1 O 0.1460(5) 0.2948(4) 0.7857(5) 0.0382(12) Uani 1 1 d . . .
O2 O 0.4881(4) 0.1068(4) 0.9317(4) 0.0208(10) Uani 1 1 d . . .
O3 O 0.5872(5) 0.3779(4) 1.2910(5) 0.0334(12) Uani 1 1 d . . .
O4 O 0.5807(4) -0.1074(4) 0.8331(4) 0.0198(9) Uani 1 1 d . . .
O5 O 0.1990(4) 0.0760(4) 0.9204(4) 0.0246(10) Uani 1 1 d . . .
O6 O 0.3555(5) -0.1557(4) 0.5768(4) 0.0314(11) Uani 1 1 d . . .
O7 O 0.2763(5) 0.0761(4) 0.6971(4) 0.0246(10) Uani 1 1 d . . .
O8 O 0.3789(5) 0.3209(4) 1.0298(4) 0.0251(10) Uani 1 1 d . . .
O9 O 0.3110(4) -0.1488(4) 0.8298(4) 0.0188(9) Uani 1 1 d . . .
O10 O 0.6811(5) 0.3870(4) 1.0750(5) 0.0312(12) Uani 1 1 d . . .
O11 O 0.4316(5) 0.3407(4) 0.7908(5) 0.0336(12) Uani 1 1 d . . .
O12 O 0.8000(5) 0.1330(4) 0.9492(4) 0.0269(11) Uani 1 1 d . . .
O13 O 0.5580(5) 0.0776(4) 0.6699(4) 0.0257(10) Uani 1 1 d . . .
N1 N 0.2021(7) 0.5017(6) 0.1083(6) 0.0456(17) Uani 1 1 d . . .
H1B H 0.2478 0.5002 0.0494 0.055 Uiso 1 1 calc R . .
N2 N 0.2522(8) 0.1009(6) 0.3967(6) 0.0448(16) Uani 1 1 d . . .
H2B H 0.3048 0.0425 0.3760 0.054 Uiso 1 1 calc R . .
C1 C -0.0303(7) 0.5038(6) 0.3924(6) 0.0244(14) Uani 1 1 d . . .
H1 H -0.1343 0.5023 0.3436 0.029 Uiso 1 1 calc R . .
C2 C -0.0207(7) 0.3834(6) 0.4716(6) 0.0222(14) Uani 1 1 d . . .
H2 H -0.1201 0.3326 0.4559 0.027 Uiso 1 1 calc R . .
C3 C 0.0571(7) 0.5063(6) 0.2963(6) 0.0236(14) Uani 1 1 d . . .
C4 C 0.1661(8) 0.6167(6) 0.3060(7) 0.0342(17) Uani 1 1 d . . .
H4 H 0.1907 0.6934 0.3780 0.041 Uiso 1 1 calc R . .
C5 C 0.2366(8) 0.6129(7) 0.2111(8) 0.0377(19) Uani 1 1 d . . .
H5 H 0.3082 0.6872 0.2177 0.045 Uiso 1 1 calc R . .
C6 C 0.1011(8) 0.3948(7) 0.0940(7) 0.0415(19) Uani 1 1 d . . .
H6 H 0.0799 0.3194 0.0211 0.050 Uiso 1 1 calc R . .
C7 C 0.0273(7) 0.3947(6) 0.1862(6) 0.0293(15) Uani 1 1 d . . .
H7 H -0.0442 0.3187 0.1754 0.035 Uiso 1 1 calc R . .
C8 C 0.0806(7) 0.2854(6) 0.4519(6) 0.0240(14) Uani 1 1 d . . .
C9 C 0.2343(8) 0.3266(7) 0.4876(7) 0.0377(18) Uani 1 1 d . . .
H9 H 0.2795 0.4176 0.5298 0.045 Uiso 1 1 calc R . .
C10 C 0.3182(8) 0.2288(8) 0.4585(7) 0.0388(18) Uani 1 1 d . . .
H10 H 0.4204 0.2538 0.4827 0.047 Uiso 1 1 calc R . .
C11 C 0.1079(9) 0.0589(7) 0.3655(8) 0.044(2) Uani 1 1 d . . .
H11 H 0.0657 -0.0330 0.3251 0.053 Uiso 1 1 calc R . .
C12 C 0.0219(8) 0.1489(6) 0.3919(7) 0.0376(18) Uani 1 1 d . . .
H12 H -0.0795 0.1181 0.3690 0.045 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'
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'
Mo Mo -1.6832 0.6857 '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
O3 Mo1 O10 105.2(2) . . ?
O3 Mo1 O8 103.1(2) . . ?
O10 Mo1 O8 101.1(2) . . ?
O3 Mo1 O9 100.6(2) . 2_657 ?
O10 Mo1 O9 96.55(19) . 2_657 ?
O8 Mo1 O9 145.44(16) . 2_657 ?
O3 Mo1 O4 88.85(18) . 2_657 ?
O10 Mo1 O4 163.68(17) . 2_657 ?
O8 Mo1 O4 83.31(16) . 2_657 ?
O9 Mo1 O4 72.32(15) 2_657 2_657 ?
O3 Mo1 O2 160.30(18) . . ?
O10 Mo1 O2 94.02(18) . . ?
O8 Mo1 O2 76.73(16) . . ?
O9 Mo1 O2 72.55(15) 2_657 . ?
O4 Mo1 O2 71.51(14) 2_657 . ?
O12 Mo2 O5 105.3(2) . 2_657 ?
O12 Mo2 O4 101.35(19) . . ?
O5 Mo2 O4 97.27(18) 2_657 . ?
O12 Mo2 O9 101.43(18) . 2_657 ?
O5 Mo2 O9 96.24(18) 2_657 2_657 ?
O4 Mo2 O9 149.34(17) . 2_657 ?
O12 Mo2 O2 98.26(19) . . ?
O5 Mo2 O2 156.49(18) 2_657 . ?
O4 Mo2 O2 77.99(16) . . ?
O9 Mo2 O2 78.67(16) 2_657 . ?
O12 Mo2 O2 174.09(18) . 2_657 ?
O5 Mo2 O2 80.65(16) 2_657 2_657 ?
O4 Mo2 O2 77.88(15) . 2_657 ?
O9 Mo2 O2 77.34(14) 2_657 2_657 ?
O2 Mo2 O2 75.84(17) . 2_657 ?
O12 Mo2 Mo4 90.14(15) . . ?
O5 Mo2 Mo4 133.38(13) 2_657 . ?
O4 Mo2 Mo4 36.13(12) . . ?
O9 Mo2 Mo4 123.94(12) 2_657 . ?
O2 Mo2 Mo4 45.30(10) . . ?
O2 Mo2 Mo4 85.86(10) 2_657 . ?
O11 Mo3 O1 106.3(2) . . ?
O11 Mo3 O8 99.3(2) . . ?
O1 Mo3 O8 102.4(2) . . ?
O11 Mo3 O7 97.91(19) . . ?
O1 Mo3 O7 101.2(2) . . ?
O8 Mo3 O7 145.43(18) . . ?
O11 Mo3 O5 163.89(19) . . ?
O1 Mo3 O5 89.75(19) . . ?
O8 Mo3 O5 77.67(16) . . ?
O7 Mo3 O5 77.51(16) . . ?
O11 Mo3 O2 93.68(18) . . ?
O1 Mo3 O2 159.93(19) . . ?
O8 Mo3 O2 75.25(16) . . ?
O7 Mo3 O2 73.92(16) . . ?
O5 Mo3 O2 70.22(14) . . ?
O6 Mo4 O13 103.7(2) . . ?
O6 Mo4 O7 100.4(2) . . ?
O13 Mo4 O7 102.61(19) . . ?
O6 Mo4 O4 100.31(19) . . ?
O13 Mo4 O4 95.40(19) . . ?
O7 Mo4 O4 148.34(17) . . ?
O6 Mo4 O2 159.70(19) . . ?
O13 Mo4 O2 96.33(17) . . ?
O7 Mo4 O2 78.27(16) . . ?
O4 Mo4 O2 74.00(15) . . ?
O6 Mo4 O9 87.09(18) . . ?
O13 Mo4 O9 164.86(18) . . ?
O7 Mo4 O9 85.55(16) . . ?
O4 Mo4 O9 71.90(15) . . ?
O2 Mo4 O9 72.61(14) . . ?
O6 Mo4 Mo2 135.33(16) . . ?
O13 Mo4 Mo2 85.43(15) . . ?
O7 Mo4 Mo2 120.43(12) . . ?
O4 Mo4 Mo2 35.03(10) . . ?
O2 Mo4 Mo2 42.19(10) . . ?
O9 Mo4 Mo2 79.43(10) . . ?
Mo2 O2 Mo4 92.51(14) . . ?
Mo2 O2 Mo1 91.58(14) . . ?
Mo4 O2 Mo1 164.7(2) . . ?
Mo2 O2 Mo2 104.16(17) . 2_657 ?
Mo4 O2 Mo2 97.46(13) . 2_657 ?
Mo1 O2 Mo2 95.80(14) . 2_657 ?
Mo2 O2 Mo3 163.7(2) . . ?
Mo4 O2 Mo3 86.87(13) . . ?
Mo1 O2 Mo3 85.09(12) . . ?
Mo2 O2 Mo3 92.08(14) 2_657 . ?
Mo2 O4 Mo4 108.84(18) . . ?
Mo2 O4 Mo1 111.98(18) . 2_657 ?
Mo4 O4 Mo1 103.37(16) . 2_657 ?
Mo2 O5 Mo3 117.0(2) 2_657 . ?
Mo4 O7 Mo3 116.3(2) . . ?
Mo1 O8 Mo3 117.3(2) . . ?
Mo2 O9 Mo1 111.14(19) 2_657 2_657 ?
Mo2 O9 Mo4 109.68(15) 2_657 . ?
Mo1 O9 Mo4 102.84(16) 2_657 . ?
C6 N1 C5 122.5(6) . . ?
C6 N1 H1B 118.7 . . ?
C5 N1 H1B 118.7 . . ?
C10 N2 C11 122.3(7) . . ?
C10 N2 H2B 118.8 . . ?
C11 N2 H2B 118.8 . . ?
C3 C1 C2 119.1(5) . 2_566 ?
C3 C1 C2 117.2(5) . . ?
C2 C1 C2 91.8(4) 2_566 . ?
C3 C1 H1 109.2 . . ?
C2 C1 H1 109.2 2_566 . ?
C2 C1 H1 109.2 . . ?
C8 C2 C1 117.7(5) . 2_566 ?
C8 C2 C1 118.7(5) . . ?
C1 C2 C1 88.2(4) 2_566 . ?
C8 C2 H2 110.2 . . ?
C1 C2 H2 110.2 2_566 . ?
C1 C2 H2 110.2 . . ?
C7 C3 C4 116.2(6) . . ?
C7 C3 C1 119.4(5) . . ?
C4 C3 C1 124.4(5) . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
N1 C5 C4 119.5(6) . . ?
N1 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
N1 C6 C7 119.8(6) . . ?
N1 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C3 121.2(6) . . ?
C6 C7 H7 119.4 . . ?
C3 C7 H7 119.4 . . ?
C12 C8 C9 117.4(6) . . ?
C12 C8 C2 119.4(6) . . ?
C9 C8 C2 123.1(5) . . ?
C10 C9 C8 118.8(6) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N2 C10 C9 119.9(7) . . ?
N2 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
N2 C11 C12 120.2(7) . . ?
N2 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C8 121.4(7) . . ?
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 O3 1.693(4) . ?
Mo1 O10 1.708(4) . ?
Mo1 O8 1.887(4) . ?
Mo1 O9 2.001(4) 2_657 ?
Mo1 O4 2.325(4) 2_657 ?
Mo1 O2 2.388(4) . ?
Mo2 O12 1.688(4) . ?
Mo2 O5 1.742(4) 2_657 ?
Mo2 O4 1.950(4) . ?
Mo2 O9 1.957(4) 2_657 ?
Mo2 O2 2.162(4) . ?
Mo2 O2 2.396(4) 2_657 ?
Mo2 Mo4 3.2156(9) . ?
Mo3 O11 1.689(4) . ?
Mo3 O1 1.699(5) . ?
Mo3 O8 1.922(4) . ?
Mo3 O7 1.935(4) . ?
Mo3 O5 2.311(4) . ?
Mo3 O2 2.423(4) . ?
Mo4 O6 1.696(4) . ?
Mo4 O13 1.713(4) . ?
Mo4 O7 1.879(4) . ?
Mo4 O4 2.003(4) . ?
Mo4 O2 2.288(4) . ?
Mo4 O9 2.342(4) . ?
O2 Mo2 2.396(4) 2_657 ?
O4 Mo1 2.325(4) 2_657 ?
O5 Mo2 1.742(4) 2_657 ?
O9 Mo2 1.957(4) 2_657 ?
O9 Mo1 2.001(4) 2_657 ?
N1 C6 1.313(8) . ?
N1 C5 1.338(8) . ?
N1 H1B 0.8600 . ?
N2 C10 1.317(8) . ?
N2 C11 1.323(9) . ?
N2 H2B 0.8600 . ?
C1 C3 1.498(8) . ?
C1 C2 1.563(7) 2_566 ?
C1 C2 1.596(8) . ?
C1 H1 0.9800 . ?
C2 C8 1.500(8) . ?
C2 C1 1.563(7) 2_566 ?
C2 H2 0.9800 . ?
C3 C7 1.394(8) . ?
C3 C4 1.398(8) . ?
C4 C5 1.364(9) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.363(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C12 1.374(8) . ?
C8 C9 1.402(9) . ?
C9 C10 1.395(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.346(9) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
