#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/17/4511742.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_4511742
loop_
_publ_author_name
'Li, Shaobin'
'Ma, Huiyuan'
'Pang, Haijun'
'Zhang, Li'
_publ_section_title
;
 Assembly of Six Polyoxometalate-Based Hybrid Compounds from a Simple
 Supramolecule to a Complicated Pseudorotaxane Framework via Tuning the pH
 of the Reaction Systems
;
_journal_issue                   9
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4450
_journal_paper_doi               10.1021/cg5005352
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'Mo6 O19,C14 H16 N4'
_chemical_formula_sum            'C14 H16 Mo6 N4 O19'
_chemical_formula_weight         1119.93
_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                113.291(5)
_cell_angle_beta                 107.492(5)
_cell_angle_gamma                92.450(5)
_cell_formula_units_Z            1
_cell_length_a                   7.741(5)
_cell_length_b                   9.604(5)
_cell_length_c                   10.200(5)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.32
_cell_volume                     652.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3256
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.890
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_density_diffrn    2.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             530.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0285
_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)+(0.0566P)²+1.9137P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                2189
_reflns_number_total             2298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5005352_si_002.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4511742--4511747.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C14 H16 Mo6 N4 O19 '
_cod_database_code               4511742
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
Mo1 Mo 0.25821(5) 0.59097(5) 0.72116(4) 0.01870(15) Uani 1 1 d .
Mo2 Mo 0.04155(5) 0.24935(4) 0.44792(4) 0.01780(15) Uani 1 1 d .
Mo3 Mo -0.18576(5) 0.48268(5) 0.63649(5) 0.01849(15) Uani 1 1 d .
O10 O 0.0841(5) 0.0703(4) 0.4156(4) 0.0265(8) Uani 1 1 d .
O7 O 0.0000 0.5000 0.5000 0.0138(9) Uani 1 2 d S
O8 O -0.3173(5) 0.4651(5) 0.7361(4) 0.0279(8) Uani 1 1 d .
O3 O 0.3566(4) 0.5984(4) 0.5729(4) 0.0202(7) Uani 1 1 d .
O2 O 0.4396(5) 0.6651(5) 0.8847(4) 0.0300(9) Uani 1 1 d .
O9 O 0.1938(5) 0.3174(4) 0.3557(4) 0.0203(7) Uani 1 1 d .
O4 O 0.0564(5) 0.5612(4) 0.7893(4) 0.0212(7) Uani 1 1 d .
C5 C 0.8247(7) -0.0695(6) 0.9660(5) 0.0210(10) Uani 1 1 d .
H5 H 0.7039 -0.1148 0.9413 0.025 Uiso 1 1 calc R
O1 O 0.1641(5) 0.7785(4) 0.7198(4) 0.0210(7) Uani 1 1 d .
O5 O 0.2480(5) 0.3750(4) 0.6417(4) 0.0214(7) Uani 1 1 d .
C4 C 0.8569(6) 0.0407(5) 0.9167(5) 0.0188(9) Uani 1 1 d .
C1 C 0.4936(6) 0.1869(6) 0.7306(6) 0.0199(10) Uani 1 1 d .
H1 H 0.4344 0.2642 0.7151 0.024 Uiso 1 1 calc R
N1 N 0.6948(5) 0.0724(5) 0.8232(5) 0.0196(8) Uani 1 1 d .
O6 O -0.1098(5) 0.2818(4) 0.5698(4) 0.0204(7) Uani 1 1 d .
C2 C 0.6562(8) 0.2085(6) 0.8328(6) 0.0263(11) Uani 1 1 d .
H2 H 0.7316 0.3036 0.9005 0.032 Uiso 1 1 calc R
C3 C 0.5508(7) -0.0408(6) 0.7077(6) 0.0266(11) Uani 1 1 d .
H3 H 0.5429 -0.1467 0.6762 0.032 Uiso 1 1 calc R
C7 C 1.0775(7) 0.2343(6) 0.8966(6) 0.0269(11) Uani 1 1 d .
H7A H 1.0054 0.2006 0.7911 0.040 Uiso 1 1 calc R
H7B H 1.2061 0.2479 0.9096 0.040 Uiso 1 1 calc R
H7C H 1.0492 0.3305 0.9558 0.040 Uiso 1 1 calc R
C6 C 1.0330(7) 0.1142(6) 0.9491(5) 0.0204(10) Uani 1 1 d .
N2 N 0.4249(7) 0.0295(7) 0.6497(7) 0.0460(13) Uani 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'
Ni Ni 0.3393 1.1124 '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
O2 Mo1 O5 105.20(17) . .
O2 Mo1 O3 104.34(18) . .
O5 Mo1 O3 89.70(15) . .
O2 Mo1 O4 102.17(18) . .
O5 Mo1 O4 88.01(15) . .
O3 Mo1 O4 153.04(15) . .
O2 Mo1 O1 101.50(17) . .
O5 Mo1 O1 153.22(15) . .
O3 Mo1 O1 85.63(15) . .
O4 Mo1 O1 84.43(15) . .
O2 Mo1 O7 176.89(14) . .
O5 Mo1 O7 77.59(10) . .
O3 Mo1 O7 76.87(11) . .
O4 Mo1 O7 76.41(11) . .
O1 Mo1 O7 75.67(10) . .
O10 Mo2 O1 104.71(17) . 2_566
O10 Mo2 O6 104.00(16) . .
O1 Mo2 O6 90.03(16) 2_566 .
O10 Mo2 O9 102.20(17) . .
O1 Mo2 O9 88.20(16) 2_566 .
O6 Mo2 O9 153.31(14) . .
O10 Mo2 O5 100.92(16) . .
O1 Mo2 O5 154.27(14) 2_566 .
O6 Mo2 O5 86.05(16) . .
O9 Mo2 O5 84.11(15) . .
O10 Mo2 O7 176.89(13) . .
O1 Mo2 O7 78.07(10) 2_566 .
O6 Mo2 O7 77.22(10) . .
O9 Mo2 O7 76.36(10) . .
O5 Mo2 O7 76.25(10) . .
O8 Mo3 O9 104.87(17) . 2_566
O8 Mo3 O4 102.46(17) . .
O9 Mo3 O4 88.75(15) 2_566 .
O8 Mo3 O3 104.36(17) . 2_566
O9 Mo3 O3 87.49(15) 2_566 2_566
O4 Mo3 O3 152.99(14) . 2_566
O8 Mo3 O6 102.30(17) . .
O9 Mo3 O6 152.80(15) 2_566 .
O4 Mo3 O6 86.60(15) . .
O3 Mo3 O6 84.64(14) 2_566 .
O8 Mo3 O7 178.06(13) . .
O9 Mo3 O7 76.97(10) 2_566 .
O4 Mo3 O7 76.89(11) . .
O3 Mo3 O7 76.20(11) 2_566 .
O6 Mo3 O7 75.87(10) . .
Mo2 O7 Mo2 180.0 2_566 .
Mo2 O7 Mo3 90.23(2) 2_566 2_566
Mo2 O7 Mo3 89.77(2) . 2_566
Mo2 O7 Mo3 89.77(2) 2_566 .
Mo2 O7 Mo3 90.23(2) . .
Mo3 O7 Mo3 180.000(1) 2_566 .
Mo2 O7 Mo1 90.35(2) 2_566 2_566
Mo2 O7 Mo1 89.65(2) . 2_566
Mo3 O7 Mo1 90.05(5) 2_566 2_566
Mo3 O7 Mo1 89.95(5) . 2_566
Mo2 O7 Mo1 89.65(2) 2_566 .
Mo2 O7 Mo1 90.35(2) . .
Mo3 O7 Mo1 89.95(5) 2_566 .
Mo3 O7 Mo1 90.05(5) . .
Mo1 O7 Mo1 180.0 2_566 .
Mo1 O3 Mo3 116.77(17) . 2_566
Mo3 O9 Mo2 116.73(17) 2_566 .
Mo3 O4 Mo1 116.65(17) . .
C4 C5 C6 121.9(5) . 2_757
Mo2 O1 Mo1 116.56(17) 2_566 .
Mo1 O5 Mo2 115.80(16) . .
C5 C4 C6 122.7(4) . .
C5 C4 N1 116.1(4) . .
C6 C4 N1 121.2(4) . .
C2 C1 N2 108.7(4) . .
C2 N1 C3 108.4(4) . .
C2 N1 C4 127.9(4) . .
C3 N1 C4 123.7(4) . .
Mo2 O6 Mo3 116.65(16) . .
C1 C2 N1 108.7(5) . .
N2 C3 N1 107.4(5) . .
C5 C6 C4 115.5(4) 2_757 .
C5 C6 C7 119.3(4) 2_757 .
C4 C6 C7 125.2(4) . .
C3 N2 C1 106.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.682(4) .
Mo1 O5 1.893(4) .
Mo1 O3 1.909(3) .
Mo1 O4 1.943(3) .
Mo1 O1 1.975(3) .
Mo1 O7 2.3300(10) .
Mo2 O10 1.685(3) .
Mo2 O1 1.870(3) 2_566
Mo2 O6 1.901(3) .
Mo2 O9 1.946(3) .
Mo2 O5 1.992(3) .
Mo2 O7 2.3104(13) .
Mo3 O8 1.685(4) .
Mo3 O9 1.895(3) 2_566
Mo3 O4 1.925(4) .
Mo3 O3 1.954(4) 2_566
Mo3 O6 1.957(3) .
Mo3 O7 2.3238(10) .
O7 Mo2 2.3104(13) 2_566
O7 Mo3 2.3238(10) 2_566
O7 Mo1 2.3300(10) 2_566
O3 Mo3 1.954(3) 2_566
O9 Mo3 1.895(3) 2_566
C5 C4 1.381(7) .
C5 C6 1.382(7) 2_757
O1 Mo2 1.870(3) 2_566
C4 C6 1.389(7) .
C4 N1 1.456(6) .
C1 C2 1.316(7) .
C1 N2 1.389(7) .
N1 C2 1.325(7) .
N1 C3 1.381(7) .
C3 N2 1.334(7) .
C7 C6 1.517(7) .
C6 C5 1.382(7) 2_757
