#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509567.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509567
loop_
_publ_author_name
'Meng, Jing-Xin'
'Lu, Ying'
'Li, Yang-Guang'
'Fu, Hai'
'Wang, En-Bo'
_publ_section_title
;
 Base-Directed Self-Assembly of Octamolybdate-Based Frameworks Decorated
 by Flexible N-Containing Ligands
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4116
_journal_paper_doi               10.1021/cg900352e
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C26 H32 Mo8 N4 O26'
_chemical_formula_weight         1584.08
_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                 100.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.460(2)
_cell_length_b                   9.974(2)
_cell_length_c                   19.618(4)
_cell_measurement_reflns_used    17920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.16
_cell_volume                     2010.5(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17920
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.511
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0304
_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)+(0.0431P)²+6.2402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3897
_reflns_number_total             4560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900352esup5.cif
_cod_data_source_block           792b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4509567
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
Mo1 Mo 0.02752(4) 0.52592(4) -0.08645(2) 0.01106(10) Uani 1 1 d .
Mo2 Mo 0.17961(4) 0.20552(4) 0.07522(2) 0.01420(11) Uani 1 1 d .
Mo3 Mo -0.07487(4) 0.23561(4) -0.04799(2) 0.01288(11) Uani 1 1 d .
Mo4 Mo 0.27743(4) 0.50200(4) 0.03646(2) 0.01276(11) Uani 1 1 d .
O1 O 0.2868(3) 0.3601(3) 0.10168(18) 0.0157(7) Uani 1 1 d .
O2 O 0.2145(4) 0.1092(4) 0.1475(2) 0.0230(8) Uani 1 1 d .
O3 O -0.2200(4) 0.1557(4) -0.0639(2) 0.0208(8) Uani 1 1 d .
O4 O 0.0814(3) 0.3899(3) -0.00036(17) 0.0125(6) Uani 1 1 d .
O5 O 0.3877(3) 0.6107(4) 0.07951(19) 0.0197(8) Uani 1 1 d .
O6 O 0.0504(3) 0.3391(4) 0.13215(18) 0.0159(7) Uani 1 1 d .
O7 O 0.0071(3) 0.1487(3) 0.03395(18) 0.0149(7) Uani 1 1 d .
O8 O 0.2637(4) 0.1373(4) 0.0173(2) 0.0248(8) Uani 1 1 d .
O9 O 0.0120(4) 0.1728(4) -0.10772(19) 0.0209(8) Uani 1 1 d .
O10 O 0.1621(3) 0.6271(3) -0.02693(17) 0.0117(6) Uani 1 1 d .
O11 O 0.1134(3) 0.4532(4) -0.14180(18) 0.0180(7) Uani 1 1 d .
O12 O 0.3493(3) 0.4306(4) -0.0261(2) 0.0220(8) Uani 1 1 d .
O13 O -0.1248(3) 0.4101(3) -0.09661(17) 0.0127(6) Uani 1 1 d .
N1 N 0.1279(5) -0.0567(5) -0.1402(3) 0.0270(11) Uani 1 1 d .
N2 N 0.6655(6) -0.2718(5) -0.3768(3) 0.0353(14) Uani 1 1 d .
C1 C 0.0775(6) -0.0908(6) -0.2060(3) 0.0273(12) Uani 1 1 d .
H1A H 0.0034 -0.0476 -0.2295 0.033 Uiso 1 1 calc R
C2 C 0.1354(5) -0.1896(6) -0.2385(3) 0.0228(11) Uani 1 1 d .
H2A H 0.1008 -0.2127 -0.2841 0.027 Uiso 1 1 calc R
C3 C 0.2453(5) -0.2548(5) -0.2033(3) 0.0167(10) Uani 1 1 d .
C4 C 0.2919(5) -0.2210(5) -0.1346(3) 0.0199(10) Uani 1 1 d .
H4A H 0.3629 -0.2661 -0.1091 0.024 Uiso 1 1 calc R
C5 C 0.2322(6) -0.1200(6) -0.1043(3) 0.0274(12) Uani 1 1 d .
H5A H 0.2645 -0.0955 -0.0586 0.033 Uiso 1 1 calc R
C6 C 0.3069(5) -0.3608(5) -0.2418(3) 0.0197(10) Uani 1 1 d .
H6A H 0.3326 -0.3195 -0.2819 0.024 Uiso 1 1 calc R
H6B H 0.2416 -0.4281 -0.2587 0.024 Uiso 1 1 calc R
C7 C 0.4247(5) -0.4305(6) -0.1996(3) 0.0213(11) Uani 1 1 d .
H7A H 0.3971 -0.4835 -0.1635 0.026 Uiso 1 1 calc R
H7B H 0.4854 -0.3633 -0.1773 0.026 Uiso 1 1 calc R
C8 C 0.4956(5) -0.5234(5) -0.2443(3) 0.0205(11) Uani 1 1 d .
H8A H 0.5611 -0.5760 -0.2142 0.025 Uiso 1 1 calc R
H8B H 0.4335 -0.5847 -0.2709 0.025 Uiso 1 1 calc R
C9 C 0.5591(5) -0.4404(5) -0.2927(3) 0.0180(10) Uani 1 1 d .
C10 C 0.5022(5) -0.4250(7) -0.3619(3) 0.0263(12) Uani 1 1 d .
H10A H 0.4273 -0.4727 -0.3804 0.032 Uiso 1 1 calc R
C11 C 0.5564(6) -0.3395(7) -0.4027(3) 0.0323(14) Uani 1 1 d .
H11A H 0.5175 -0.3281 -0.4490 0.039 Uiso 1 1 calc R
C12 C 0.7252(7) -0.2855(7) -0.3109(4) 0.0334(14) Uani 1 1 d .
H12A H 0.8010 -0.2378 -0.2942 0.040 Uiso 1 1 calc R
C13 C 0.6740(5) -0.3711(6) -0.2676(3) 0.0229(11) Uani 1 1 d .
H13A H 0.7160 -0.3824 -0.2218 0.027 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'
Mo Mo -1.6832 0.6857 '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'
N N 0.0061 0.0033 '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'
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
O11 Mo1 O6 104.77(17) . 3_565
O11 Mo1 O10 101.35(16) . .
O6 Mo1 O10 97.19(15) 3_565 .
O11 Mo1 O13 101.64(16) . .
O6 Mo1 O13 96.39(15) 3_565 .
O10 Mo1 O13 149.25(14) . .
O11 Mo1 O4 98.07(15) . .
O6 Mo1 O4 157.15(14) 3_565 .
O10 Mo1 O4 78.56(13) . .
O13 Mo1 O4 78.24(13) . .
O11 Mo1 O4 173.60(15) . 3_565
O6 Mo1 O4 81.61(14) 3_565 3_565
O10 Mo1 O4 77.01(12) . 3_565
O13 Mo1 O4 77.86(12) . 3_565
O4 Mo1 O4 75.56(13) . 3_565
O11 Mo1 Mo4 89.71(12) . .
O6 Mo1 Mo4 133.04(12) 3_565 .
O10 Mo1 Mo4 35.85(10) . .
O13 Mo1 Mo4 124.55(10) . .
O4 Mo1 Mo4 46.35(9) . .
O4 Mo1 Mo4 85.42(8) 3_565 .
O2 Mo2 O8 105.94(19) . .
O2 Mo2 O7 102.91(17) . .
O8 Mo2 O7 99.36(18) . .
O2 Mo2 O1 101.86(17) . .
O8 Mo2 O1 98.77(17) . .
O7 Mo2 O1 143.76(14) . .
O2 Mo2 O6 88.63(16) . .
O8 Mo2 O6 165.40(16) . .
O7 Mo2 O6 77.70(14) . .
O1 Mo2 O6 76.88(14) . .
O2 Mo2 O4 157.97(16) . .
O8 Mo2 O4 96.09(16) . .
O7 Mo2 O4 73.35(13) . .
O1 Mo2 O4 73.73(13) . .
O6 Mo2 O4 69.34(11) . .
O3 Mo3 O9 105.77(19) . .
O3 Mo3 O7 100.95(17) . .
O9 Mo3 O7 101.44(17) . .
O3 Mo3 O13 100.16(16) . .
O9 Mo3 O13 96.61(16) . .
O7 Mo3 O13 147.20(14) . .
O3 Mo3 O4 158.57(16) . .
O9 Mo3 O4 95.38(15) . .
O7 Mo3 O4 77.71(13) . .
O13 Mo3 O4 73.49(13) . .
O3 Mo3 O10 87.07(15) . 3_565
O9 Mo3 O10 164.41(15) . 3_565
O7 Mo3 O10 84.32(14) . 3_565
O13 Mo3 O10 71.99(12) . 3_565
O4 Mo3 O10 71.50(11) . 3_565
O5 Mo4 O12 105.97(18) . .
O5 Mo4 O1 101.37(16) . .
O12 Mo4 O1 101.47(17) . .
O5 Mo4 O10 100.74(16) . .
O12 Mo4 O10 96.25(16) . .
O1 Mo4 O10 146.50(14) . .
O5 Mo4 O13 88.50(15) . 3_565
O12 Mo4 O13 163.02(15) . 3_565
O1 Mo4 O13 83.87(13) . 3_565
O10 Mo4 O13 71.87(12) . 3_565
O5 Mo4 O4 160.44(15) . .
O12 Mo4 O4 93.30(15) . .
O1 Mo4 O4 77.45(13) . .
O10 Mo4 O4 73.32(12) . .
O13 Mo4 O4 71.95(12) 3_565 .
O5 Mo4 Mo1 135.25(13) . .
O12 Mo4 Mo1 84.13(13) . .
O1 Mo4 Mo1 119.54(10) . .
O10 Mo4 Mo1 34.55(9) . .
O13 Mo4 Mo1 79.27(8) 3_565 .
O4 Mo4 Mo1 42.10(8) . .
Mo4 O1 Mo2 117.55(17) . .
Mo1 O4 Mo3 92.33(12) . .
Mo1 O4 Mo4 91.55(12) . .
Mo3 O4 Mo4 163.78(16) . .
Mo1 O4 Mo1 104.44(13) . 3_565
Mo3 O4 Mo1 97.32(12) . 3_565
Mo4 O4 Mo1 96.94(12) . 3_565
Mo1 O4 Mo2 163.58(16) . .
Mo3 O4 Mo2 85.97(11) . .
Mo4 O4 Mo2 85.87(11) . .
Mo1 O4 Mo2 91.96(11) 3_565 .
Mo1 O6 Mo2 117.09(17) 3_565 .
Mo3 O7 Mo2 117.74(17) . .
Mo1 O10 Mo4 109.60(15) . .
Mo1 O10 Mo3 111.26(14) . 3_565
Mo4 O10 Mo3 103.74(14) . 3_565
Mo1 O13 Mo3 109.32(16) . .
Mo1 O13 Mo4 110.51(14) . 3_565
Mo3 O13 Mo4 103.17(14) . 3_565
C5 N1 C1 121.3(5) . .
C12 N2 C11 121.9(5) . .
N1 C1 C2 120.0(6) . .
N1 C1 H1A 120.0 . .
C2 C1 H1A 120.0 . .
C1 C2 C3 120.1(5) . .
C1 C2 H2A 119.9 . .
C3 C2 H2A 119.9 . .
C4 C3 C2 118.5(5) . .
C4 C3 C6 123.4(5) . .
C2 C3 C6 118.1(5) . .
C5 C4 C3 119.5(5) . .
C5 C4 H4A 120.3 . .
C3 C4 H4A 120.3 . .
N1 C5 C4 120.5(5) . .
N1 C5 H5A 119.7 . .
C4 C5 H5A 119.7 . .
C3 C6 C7 115.2(4) . .
C3 C6 H6A 108.5 . .
C7 C6 H6A 108.5 . .
C3 C6 H6B 108.5 . .
C7 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
C6 C7 C8 112.9(4) . .
C6 C7 H7A 109.0 . .
C8 C7 H7A 109.0 . .
C6 C7 H7B 109.0 . .
C8 C7 H7B 109.0 . .
H7A C7 H7B 107.8 . .
C9 C8 C7 110.0(4) . .
C9 C8 H8A 109.7 . .
C7 C8 H8A 109.7 . .
C9 C8 H8B 109.7 . .
C7 C8 H8B 109.7 . .
H8A C8 H8B 108.2 . .
C10 C9 C13 118.4(5) . .
C10 C9 C8 121.4(5) . .
C13 C9 C8 120.1(5) . .
C11 C10 C9 119.7(6) . .
C11 C10 H10A 120.2 . .
C9 C10 H10A 120.2 . .
N2 C11 C10 120.6(6) . .
N2 C11 H11A 119.7 . .
C10 C11 H11A 119.7 . .
N2 C12 C13 119.6(6) . .
N2 C12 H12A 120.2 . .
C13 C12 H12A 120.2 . .
C12 C13 C9 119.8(6) . .
C12 C13 H13A 120.1 . .
C9 C13 H13A 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O11 1.696(3) .
Mo1 O6 1.734(4) 3_565
Mo1 O10 1.936(3) .
Mo1 O13 1.948(3) .
Mo1 O4 2.157(3) .
Mo1 O4 2.373(3) 3_565
Mo1 Mo4 3.2163(12) .
Mo2 O2 1.695(4) .
Mo2 O8 1.704(4) .
Mo2 O7 1.920(3) .
Mo2 O1 1.920(3) .
Mo2 O6 2.327(3) .
Mo2 O4 2.463(3) .
Mo3 O3 1.690(4) .
Mo3 O9 1.729(4) .
Mo3 O7 1.885(3) .
Mo3 O13 2.006(3) .
Mo3 O4 2.312(3) .
Mo3 O10 2.317(3) 3_565
Mo4 O5 1.689(4) .
Mo4 O12 1.710(4) .
Mo4 O1 1.898(3) .
Mo4 O10 2.000(3) .
Mo4 O13 2.327(3) 3_565
Mo4 O4 2.328(3) .
O4 Mo1 2.373(3) 3_565
O6 Mo1 1.734(4) 3_565
O10 Mo3 2.317(3) 3_565
O13 Mo4 2.327(3) 3_565
N1 C5 1.341(8) .
N1 C1 1.343(8) .
N2 C12 1.333(9) .
N2 C11 1.341(9) .
C1 C2 1.374(8) .
C1 H1A 0.9300 .
C2 C3 1.387(8) .
C2 H2A 0.9300 .
C3 C4 1.387(7) .
C3 C6 1.511(7) .
C4 C5 1.377(8) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 C7 1.518(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.555(7) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.505(7) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.384(7) .
C9 C13 1.395(8) .
C10 C11 1.365(9) .
C10 H10A 0.9300 .
C11 H11A 0.9300 .
C12 C13 1.381(8) .
C12 H12A 0.9300 .
C13 H13A 0.9300 .
