#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:26:43 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179631 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/95/4509563.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_4509563
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            'C14 H18 Mo4 N4 O14'
_chemical_formula_weight         850.08
_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                85.06(3)
_cell_angle_beta                 85.38(3)
_cell_angle_gamma                78.61(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6547(19)
_cell_length_b                   10.657(2)
_cell_length_c                   11.918(2)
_cell_measurement_reflns_used    11142
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.18
_cell_volume                     1195.1(4)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku RAXIS 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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0939
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11142
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.646
_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    2.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.208
_refine_diff_density_min         -3.049
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0974P)²+7.2162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                3473
_reflns_number_total             5300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900352esup1.cif
_cod_data_source_block           141a
_cod_database_code               4509563
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 0.07656(10) 0.53051(9) 0.22615(7) 0.0292(2) Uani 1 1 d .
Mo2 Mo -0.24174(10) 0.67824(9) 0.16857(8) 0.0308(3) Uani 1 1 d .
Mo3 Mo 0.10596(9) 0.60927(8) -0.04836(7) 0.0266(2) Uani 1 1 d .
Mo4 Mo 0.39839(10) 0.40897(9) 0.03710(8) 0.0305(3) Uani 1 1 d .
O1 O 0.2086(8) 0.4967(7) 0.0960(6) 0.0321(16) Uani 1 1 d .
O2 O 0.1190(9) 0.6682(8) 0.2568(7) 0.0392(19) Uani 1 1 d .
O3 O -0.0420(7) 0.5972(6) 0.0708(5) 0.0225(14) Uani 1 1 d .
O4 O 0.5602(8) 0.4084(8) -0.0501(7) 0.0385(19) Uani 1 1 d .
O5 O 0.2691(8) 0.5084(7) -0.1125(6) 0.0341(17) Uani 1 1 d .
O6 O 0.1537(9) 0.7501(8) -0.0305(7) 0.0359(18) Uani 1 1 d .
O7 O 0.3321(8) 0.2807(7) -0.0199(6) 0.0333(17) Uani 1 1 d .
O8 O 0.0006(8) 0.6439(7) -0.1642(6) 0.0286(15) Uani 1 1 d .
O9 O -0.1219(9) 0.5723(8) 0.2763(6) 0.0371(18) Uani 1 1 d .
O10 O -0.3936(9) 0.6892(8) 0.2527(7) 0.042(2) Uani 1 1 d .
O11 O -0.1928(9) 0.8219(8) 0.1702(8) 0.042(2) Uani 1 1 d .
O12 O 0.4498(9) 0.3356(8) 0.1637(7) 0.0372(18) Uani 1 1 d .
O13 O 0.1477(9) 0.4205(8) 0.3297(7) 0.0400(19) Uani 1 1 d .
C1 C -0.6124(14) 0.6136(13) 0.6301(11) 0.046(3) Uani 1 1 d .
H1A H -0.5794 0.6039 0.7021 0.055 Uiso 1 1 calc R
N1 N -0.7270(12) 0.5782(10) 0.6005(9) 0.044(3) Uani 1 1 d .
C2 C -0.7455(15) 0.6120(13) 0.4880(11) 0.048(3) Uani 1 1 d .
H2A H -0.8193 0.6003 0.4469 0.057 Uiso 1 1 calc R
C3 C -0.6316(16) 0.6669(13) 0.4492(11) 0.049(3) Uani 1 1 d .
H3A H -0.6123 0.6988 0.3757 0.059 Uiso 1 1 calc R
N2 N -0.5533(11) 0.6655(10) 0.5382(8) 0.039(2) Uani 1 1 d .
C4 C -0.4245(14) 0.7238(14) 0.5370(14) 0.053(3) Uani 1 1 d .
H4A H -0.3556 0.6894 0.4782 0.064 Uiso 1 1 calc R
H4B H -0.3818 0.7034 0.6088 0.064 Uiso 1 1 calc R
C5 C -0.4672(14) 0.8676(12) 0.5154(11) 0.043(3) Uani 1 1 d .
C6 C -0.5653(18) 0.9376(15) 0.5868(14) 0.068(5) Uani 1 1 d .
H6A H -0.6082 0.8957 0.6476 0.081 Uiso 1 1 calc R
C7 C -0.3990(15) 0.9320(13) 0.4302(12) 0.049(3) Uani 1 1 d .
H7A H -0.3280 0.8865 0.3838 0.059 Uiso 1 1 calc R
C8 C 0.2562(16) 1.1099(14) 0.2041(13) 0.057(4) Uani 1 1 d .
H8A H 0.2283 1.1949 0.2215 0.068 Uiso 1 1 calc R
N3 N 0.3860(11) 1.0564(11) 0.1665(11) 0.050(3) Uani 1 1 d .
C9 C 0.3820(17) 0.9339(15) 0.1486(14) 0.064(4) Uani 1 1 d .
H9A H 0.4581 0.8734 0.1222 0.076 Uiso 1 1 calc R
C10 C 0.2519(19) 0.9143(16) 0.1749(14) 0.065(4) Uani 1 1 d .
H10A H 0.2201 0.8385 0.1685 0.078 Uiso 1 1 calc R
N4 N 0.1725(11) 1.0246(10) 0.2131(9) 0.042(2) Uani 1 1 d .
C11 C 0.0249(16) 1.0457(16) 0.2553(12) 0.056(4) Uani 1 1 d .
H11A H -0.0232 0.9882 0.2213 0.068 Uiso 1 1 calc R
H11B H -0.0202 1.1330 0.2334 0.068 Uiso 1 1 calc R
C12 C 0.0098(13) 1.0233(13) 0.3825(12) 0.049(3) Uani 1 1 d .
C13 C 0.0214(17) 1.1157(14) 0.4527(14) 0.059(4) Uani 1 1 d .
H13A H 0.0371 1.1951 0.4216 0.071 Uiso 1 1 calc R
C14 C -0.0106(16) 0.9064(14) 0.4331(13) 0.055(4) Uani 1 1 d .
H14A H -0.0171 0.8410 0.3880 0.066 Uiso 1 1 calc R
OW1 O 0.6652(11) 1.0842(10) 0.1325(10) 0.069(3) 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'
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 O13 104.2(4) . .
O2 Mo1 O9 96.7(4) . .
O13 Mo1 O9 103.4(4) . .
O2 Mo1 O1 98.0(4) . .
O13 Mo1 O1 104.0(4) . .
O9 Mo1 O1 144.6(3) . .
O2 Mo1 O3 100.5(3) . .
O13 Mo1 O3 155.4(3) . .
O9 Mo1 O3 73.6(3) . .
O1 Mo1 O3 72.2(3) . .
O2 Mo1 O8 172.1(3) . 2_565
O13 Mo1 O8 83.7(3) . 2_565
O9 Mo1 O8 80.4(3) . 2_565
O1 Mo1 O8 80.6(3) . 2_565
O3 Mo1 O8 71.7(2) . 2_565
O11 Mo2 O10 105.3(4) . .
O11 Mo2 O9 102.3(4) . .
O10 Mo2 O9 95.8(4) . .
O11 Mo2 O7 95.1(4) . 2_565
O10 Mo2 O7 97.3(4) . 2_565
O9 Mo2 O7 154.7(3) . 2_565
O11 Mo2 O5 161.6(4) . 2_565
O10 Mo2 O5 91.0(4) . 2_565
O9 Mo2 O5 84.1(3) . 2_565
O7 Mo2 O5 74.1(3) 2_565 2_565
O11 Mo2 O3 91.9(3) . .
O10 Mo2 O3 161.6(3) . .
O9 Mo2 O3 74.0(3) . .
O7 Mo2 O3 87.3(3) 2_565 .
O5 Mo2 O3 73.1(2) 2_565 .
O6 Mo3 O8 104.0(4) . .
O6 Mo3 O5 104.7(4) . .
O8 Mo3 O5 101.0(3) . .
O6 Mo3 O3 103.6(3) . .
O8 Mo3 O3 99.0(3) . .
O5 Mo3 O3 140.0(3) . .
O6 Mo3 O1 97.9(3) . .
O8 Mo3 O1 157.9(3) . .
O5 Mo3 O1 75.5(3) . .
O3 Mo3 O1 73.1(3) . .
O6 Mo3 O3 178.4(3) . 2_565
O8 Mo3 O3 77.5(3) . 2_565
O5 Mo3 O3 74.5(3) . 2_565
O3 Mo3 O3 76.4(3) . 2_565
O1 Mo3 O3 80.6(3) . 2_565
O12 Mo4 O4 105.3(4) . .
O12 Mo4 O7 100.2(4) . .
O4 Mo4 O7 100.8(4) . .
O12 Mo4 O1 95.6(4) . .
O4 Mo4 O1 151.4(3) . .
O7 Mo4 O1 94.4(3) . .
O12 Mo4 O4 100.8(4) . 2_665
O4 Mo4 O4 76.7(4) . 2_665
O7 Mo4 O4 158.8(3) . 2_665
O1 Mo4 O4 80.3(3) . 2_665
O12 Mo4 O5 164.8(3) . .
O4 Mo4 O5 89.9(3) . .
O7 Mo4 O5 75.3(3) . .
O1 Mo4 O5 70.7(3) . .
O4 Mo4 O5 83.7(3) 2_665 .
O12 Mo4 Mo4 106.5(3) . 2_665
O4 Mo4 Mo4 41.6(3) . 2_665
O7 Mo4 Mo4 138.3(2) . 2_665
O1 Mo4 Mo4 113.8(2) . 2_665
O4 Mo4 Mo4 35.1(2) 2_665 2_665
O5 Mo4 Mo4 85.6(2) . 2_665
Mo1 O1 Mo4 147.2(4) . .
Mo1 O1 Mo3 106.2(3) . .
Mo4 O1 Mo3 106.5(3) . .
Mo3 O3 Mo2 152.2(4) . .
Mo3 O3 Mo1 104.2(3) . .
Mo2 O3 Mo1 93.6(2) . .
Mo3 O3 Mo3 103.6(3) . 2_565
Mo2 O3 Mo3 95.7(2) . 2_565
Mo1 O3 Mo3 95.2(3) . 2_565
Mo4 O4 Mo4 103.3(4) . 2_665
Mo3 O5 Mo2 115.6(4) . 2_565
Mo3 O5 Mo4 106.1(3) . .
Mo2 O5 Mo4 92.2(3) 2_565 .
Mo4 O7 Mo2 117.0(4) . 2_565
Mo3 O8 Mo1 115.4(4) . 2_565
Mo2 O9 Mo1 114.9(4) . .
N1 C1 N2 107.2(11) . .
N1 C1 H1A 126.4 . .
N2 C1 H1A 126.4 . .
C1 N1 C2 110.2(10) . .
C3 C2 N1 105.3(11) . .
C3 C2 H2A 127.4 . .
N1 C2 H2A 127.4 . .
N2 C3 C2 106.8(11) . .
N2 C3 H3A 126.6 . .
C2 C3 H3A 126.6 . .
C1 N2 C3 110.4(10) . .
C1 N2 C4 124.0(11) . .
C3 N2 C4 125.4(11) . .
N2 C4 C5 108.8(11) . .
N2 C4 H4A 109.9 . .
C5 C4 H4A 109.9 . .
N2 C4 H4B 109.9 . .
C5 C4 H4B 109.9 . .
H4A C4 H4B 108.3 . .
C6 C5 C7 118.5(12) . .
C6 C5 C4 120.6(12) . .
C7 C5 C4 120.6(13) . .
C7 C6 C5 120.9(13) 2_476 .
C7 C6 H6A 119.6 2_476 .
C5 C6 H6A 119.6 . .
C6 C7 C5 120.5(13) 2_476 .
C6 C7 H7A 119.8 2_476 .
C5 C7 H7A 119.8 . .
N4 C8 N3 110.2(13) . .
N4 C8 H8A 124.9 . .
N3 C8 H8A 124.9 . .
C8 N3 C9 106.6(12) . .
C10 C9 N3 108.6(14) . .
C10 C9 H9A 125.7 . .
N3 C9 H9A 125.7 . .
C9 C10 N4 108.0(14) . .
C9 C10 H10A 126.0 . .
N4 C10 H10A 126.0 . .
C8 N4 C10 106.5(12) . .
C8 N4 C11 126.3(12) . .
C10 N4 C11 127.2(12) . .
N4 C11 C12 111.8(12) . .
N4 C11 H11A 109.3 . .
C12 C11 H11A 109.3 . .
N4 C11 H11B 109.3 . .
C12 C11 H11B 109.3 . .
H11A C11 H11B 107.9 . .
C13 C12 C14 116.9(14) . .
C13 C12 C11 122.0(13) . .
C14 C12 C11 121.1(14) . .
C14 C13 C12 121.5(13) 2_576 .
C14 C13 H13A 119.3 2_576 .
C12 C13 H13A 119.3 . .
C13 C14 C12 121.6(14) 2_576 .
C13 C14 H14A 119.2 2_576 .
C12 C14 H14A 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 1.676(8) .
Mo1 O13 1.714(8) .
Mo1 O9 1.937(8) .
Mo1 O1 1.938(7) .
Mo1 O3 2.244(7) .
Mo1 O8 2.330(7) 2_565
Mo2 O11 1.691(8) .
Mo2 O10 1.698(8) .
Mo2 O9 1.933(8) .
Mo2 O7 2.014(8) 2_565
Mo2 O5 2.221(8) 2_565
Mo2 O3 2.231(7) .
Mo3 O6 1.689(8) .
Mo3 O8 1.751(7) .
Mo3 O5 1.871(8) .
Mo3 O3 1.946(7) .
Mo3 O1 2.198(8) .
Mo3 O3 2.441(6) 2_565
Mo4 O12 1.703(8) .
Mo4 O4 1.804(8) .
Mo4 O7 1.820(8) .
Mo4 O1 1.989(8) .
Mo4 O4 2.083(8) 2_665
Mo4 O5 2.317(7) .
Mo4 Mo4 3.053(2) 2_665
O3 Mo3 2.441(6) 2_565
O4 Mo4 2.083(8) 2_665
O5 Mo2 2.221(8) 2_565
O7 Mo2 2.014(8) 2_565
O8 Mo1 2.330(7) 2_565
C1 N1 1.320(16) .
C1 N2 1.323(15) .
C1 H1A 0.9300 .
N1 C2 1.375(16) .
C2 C3 1.374(18) .
C2 H2A 0.9300 .
C3 N2 1.349(16) .
C3 H3A 0.9300 .
N2 C4 1.494(15) .
C4 C5 1.511(18) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.370(19) .
C5 C7 1.373(17) .
C6 C7 1.37(2) 2_476
C6 H6A 0.9300 .
C7 C6 1.37(2) 2_476
C7 H7A 0.9300 .
C8 N4 1.322(17) .
C8 N3 1.329(18) .
C8 H8A 0.9300 .
N3 C9 1.35(2) .
C9 C10 1.32(2) .
C9 H9A 0.9300 .
C10 N4 1.362(19) .
C10 H10A 0.9300 .
N4 C11 1.453(17) .
C11 C12 1.513(19) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.37(2) .
C12 C14 1.380(18) .
C13 C14 1.36(2) 2_576
C13 H13A 0.9300 .
C14 C13 1.36(2) 2_576
C14 H14A 0.9300 .
