#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:04:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179438 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/35/4333563.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_4333563
loop_
_publ_author_name
'Yun Gong'
'Tao Wu'
'Peng Gang Jiang'
'Jian Hua Lin'
'Yong Xi Yang'
_publ_contact_author_address
;
 Department of Chemistry 
 College of Chemistry and Chemical Engineering
 Chongqing University
 Chongqing, 400030
 P. R. China
;
_publ_contact_author_email       jhlin@cqu.edu.cn
_publ_contact_author_fax         +86-023-65102316
_publ_contact_author_name        'Prof. Jianhua Lin'
_publ_contact_author_phone       +86-023-65102316
_publ_section_title
;
 Octamolybdate-Based Metal-Organic Framework with Unsaturated Coordinated
 Metal Center As Electrocatalyst for Generating Hydrogen from Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              777
_journal_page_last               784
_journal_paper_doi               10.1021/ic3018858
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C8 H22 Cu3 Mo8 N16 O30'
_chemical_formula_weight         1780.56
_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                116.636(2)
_cell_angle_beta                 100.8770(10)
_cell_angle_gamma                94.3770(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9318(8)
_cell_length_b                   11.1272(9)
_cell_length_c                   11.2538(10)
_cell_measurement_temperature    298(2)
_cell_volume                     965.17(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4749
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    4.241
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.063
_exptl_crystal_description       block
_exptl_crystal_F_000             845
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0284
_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)+(0.0347P)²+0.2533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                2929
_reflns_number_total             3331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3018858_si_002_1.cif
_cod_data_source_block           111214d
_cod_original_cell_volume        965.17(14)
_cod_database_code               4333563
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
Cu1 Cu 0.68041(8) 0.32503(6) 0.13577(6) 0.01901(16) Uani 1 1 d .
Cu2 Cu 0.5000 0.0000 0.0000 0.0182(2) Uani 1 2 d S
Mo1 Mo 0.82528(5) 0.90212(4) 0.38076(4) 0.01221(12) Uani 1 1 d .
Mo2 Mo 1.14318(5) 0.90837(4) 0.26702(4) 0.01452(12) Uani 1 1 d .
Mo3 Mo 0.96781(5) 0.61272(4) 0.31499(4) 0.01340(12) Uani 1 1 d .
Mo4 Mo 1.08500(5) 1.22240(4) 0.37784(4) 0.01569(12) Uani 1 1 d .
N1 N 0.8106(5) 0.5494(4) 0.0996(4) 0.0182(10) Uani 1 1 d .
N2 N 0.6988(5) 0.4316(4) 0.0348(4) 0.0172(9) Uani 1 1 d .
N3 N 0.6694(5) 0.5375(4) -0.0867(4) 0.0168(9) Uani 1 1 d .
N4 N 0.6025(5) 0.5738(5) -0.1863(5) 0.0285(12) Uani 1 1 d .
H4A H 0.5190 0.5239 -0.2476 0.034 Uiso 1 1 calc R
H4B H 0.6449 0.6460 -0.1860 0.034 Uiso 1 1 calc R
N5 N 0.6331(5) 0.2542(4) 0.2579(4) 0.0166(9) Uani 1 1 d .
N6 N 0.5713(5) 0.1186(4) 0.2078(4) 0.0153(9) Uani 1 1 d .
N7 N 0.5750(5) 0.2298(4) 0.4243(4) 0.0150(9) Uani 1 1 d .
N8 N 0.5499(5) 0.2647(5) 0.5552(4) 0.0239(11) Uani 1 1 d .
H8A H 0.5739 0.3484 0.6187 0.029 Uiso 1 1 calc R
H8B H 0.5107 0.2021 0.5713 0.029 Uiso 1 1 calc R
O1 O 1.0028(4) 0.7850(3) 0.2978(3) 0.0155(7) Uani 1 1 d .
O2 O 0.9948(4) 1.0309(3) 0.3934(3) 0.0149(7) Uani 1 1 d .
O3 O 0.7944(4) 0.7488(3) 0.4074(3) 0.0158(8) Uani 1 1 d .
O4 O 0.7011(4) 0.8514(4) 0.2248(4) 0.0223(8) Uani 1 1 d .
O5 O 0.7357(4) 1.0180(4) 0.4982(4) 0.0186(8) Uani 1 1 d .
O6 O 1.2270(4) 1.0940(4) 0.3199(4) 0.0187(8) Uani 1 1 d .
O7 O 1.0398(4) 0.8621(4) 0.1043(4) 0.0271(9) Uani 1 1 d .
O8 O 1.3038(4) 0.8318(4) 0.2465(4) 0.0217(8) Uani 1 1 d .
O9 O 0.8331(4) 0.4722(4) 0.2863(4) 0.0234(9) Uani 1 1 d .
O10 O 1.0535(4) 0.6916(4) 0.5016(3) 0.0170(8) Uani 1 1 d .
O11 O 1.1141(4) 0.5449(4) 0.2474(4) 0.0273(9) Uani 1 1 d .
O12 O 0.9555(4) 1.1700(4) 0.2253(4) 0.0274(9) Uani 1 1 d .
O13 O 1.2059(5) 1.3625(4) 0.4032(4) 0.0285(9) Uani 1 1 d .
O14 O 0.5694(5) 0.1586(3) -0.0144(3) 0.0263(9) Uani 1 1 d .
H14 H 0.5484 0.1539 -0.0934 0.032 Uiso 1 1 d R
O15 O 0.2530(5) 0.1081(5) 0.0524(5) 0.0544(14) Uani 1 1 d .
H15A H 0.2406 0.1046 0.1240 0.065 Uiso 1 1 d R
H15B H 0.1674 0.1163 0.0112 0.065 Uiso 1 1 d R
C1 C 0.6156(6) 0.4280(5) -0.0753(5) 0.0209(12) Uani 1 1 d .
H1 H 0.5314 0.3599 -0.1368 0.025 Uiso 1 1 calc R
C2 C 0.7916(6) 0.6104(5) 0.0221(5) 0.0197(12) Uani 1 1 d .
H2 H 0.8528 0.6909 0.0398 0.024 Uiso 1 1 calc R
C3 C 0.5388(6) 0.1056(5) 0.3106(5) 0.0163(11) Uani 1 1 d .
H3 H 0.4975 0.0241 0.3063 0.020 Uiso 1 1 calc R
C4 C 0.6355(6) 0.3193(5) 0.3883(5) 0.0162(11) Uani 1 1 d .
H4 H 0.6728 0.4121 0.4465 0.019 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'
Cu Cu 0.3201 1.2651 '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
O14 Cu1 O9 166.68(17) . .
O14 Cu1 N5 88.40(16) . .
O9 Cu1 N5 90.50(16) . .
O14 Cu1 N2 98.12(16) . .
O9 Cu1 N2 85.97(16) . .
N5 Cu1 N2 165.93(17) . .
O14 Cu2 O14 180 2_655 .
O14 Cu2 N6 92.76(15) 2_655 .
O14 Cu2 N6 87.24(15) . .
O14 Cu2 N6 87.24(15) 2_655 2_655
O14 Cu2 N6 92.76(15) . 2_655
N6 Cu2 N6 180 . 2_655
O14 Cu2 O15 94.36(16) 2_655 .
O14 Cu2 O15 85.64(16) . .
N6 Cu2 O15 79.06(16) . .
N6 Cu2 O15 100.94(16) 2_655 .
O4 Mo1 O5 104.00(16) . .
O4 Mo1 O3 102.85(16) . .
O5 Mo1 O3 102.49(16) . .
O4 Mo1 O2 104.99(16) . .
O5 Mo1 O2 98.86(16) . .
O3 Mo1 O2 139.33(14) . .
O4 Mo1 O1 95.47(15) . .
O5 Mo1 O1 160.25(14) . .
O3 Mo1 O1 75.84(13) . .
O2 Mo1 O1 72.54(13) . .
O4 Mo1 O2 178.39(15) . 2_776
O5 Mo1 O2 76.82(13) . 2_776
O3 Mo1 O2 75.59(13) . 2_776
O2 Mo1 O2 76.17(14) . 2_776
O1 Mo1 O2 83.79(12) . 2_776
O7 Mo2 O8 105.05(18) . .
O7 Mo2 O6 98.34(17) . .
O8 Mo2 O6 102.04(16) . .
O7 Mo2 O1 95.72(16) . .
O8 Mo2 O1 103.52(16) . .
O6 Mo2 O1 146.39(14) . .
O7 Mo2 O2 102.28(16) . .
O8 Mo2 O2 152.62(15) . .
O6 Mo2 O2 75.40(13) . .
O1 Mo2 O2 71.84(13) . .
O7 Mo2 O5 173.98(16) . 2_776
O8 Mo2 O5 80.88(15) . 2_776
O6 Mo2 O5 81.21(13) . 2_776
O1 Mo2 O5 81.68(13) . 2_776
O2 Mo2 O5 71.76(12) . 2_776
O11 Mo3 O9 105.47(18) . .
O11 Mo3 O10 102.98(17) . .
O9 Mo3 O10 102.01(16) . .
O11 Mo3 O1 96.42(17) . .
O9 Mo3 O1 146.87(16) . .
O10 Mo3 O1 96.80(14) . .
O11 Mo3 O3 167.03(16) . .
O9 Mo3 O3 87.12(15) . .
O10 Mo3 O3 76.81(13) . .
O1 Mo3 O3 70.86(13) . .
O11 Mo3 N1 91.97(17) . .
O9 Mo3 N1 77.20(15) . .
O10 Mo3 N1 164.57(15) . .
O1 Mo3 N1 77.49(14) . .
O3 Mo3 N1 87.77(13) . .
O12 Mo4 O13 105.55(19) . .
O12 Mo4 O6 100.17(17) . .
O13 Mo4 O6 96.44(17) . .
O12 Mo4 O10 97.54(16) . 2_776
O13 Mo4 O10 101.43(17) . 2_776
O6 Mo4 O10 150.40(14) . 2_776
O12 Mo4 O2 92.46(16) . .
O13 Mo4 O2 160.37(16) . .
O6 Mo4 O2 72.28(13) . .
O10 Mo4 O2 83.47(13) 2_776 .
O12 Mo4 O3 162.58(16) . 2_776
O13 Mo4 O3 91.22(15) . 2_776
O6 Mo4 O3 82.21(13) . 2_776
O10 Mo4 O3 74.06(12) 2_776 2_776
O2 Mo4 O3 71.69(12) . 2_776
C2 N1 N2 106.8(4) . .
C2 N1 Mo3 133.0(3) . .
N2 N1 Mo3 119.8(3) . .
C1 N2 N1 107.6(4) . .
C1 N2 Cu1 134.7(4) . .
N1 N2 Cu1 117.0(3) . .
C1 N3 C2 106.6(4) . .
C1 N3 N4 126.2(4) . .
C2 N3 N4 127.0(4) . .
N3 N4 H4A 120.0 . .
N3 N4 H4B 120.0 . .
H4A N4 H4B 120.0 . .
C4 N5 N6 108.4(4) . .
C4 N5 Cu1 130.0(4) . .
N6 N5 Cu1 121.2(3) . .
C3 N6 N5 106.9(4) . .
C3 N6 Cu2 133.0(4) . .
N5 N6 Cu2 117.7(3) . .
C4 N7 C3 106.7(4) . .
C4 N7 N8 124.8(4) . .
C3 N7 N8 128.4(4) . .
N7 N8 H8A 120.0 . .
N7 N8 H8B 120.0 . .
H8A N8 H8B 120.0 . .
Mo2 O1 Mo3 147.36(18) . .
Mo2 O1 Mo1 105.66(15) . .
Mo3 O1 Mo1 105.91(15) . .
Mo1 O2 Mo2 106.73(15) . .
Mo1 O2 Mo4 150.75(17) . .
Mo2 O2 Mo4 92.33(12) . .
Mo1 O2 Mo1 103.83(14) . 2_776
Mo2 O2 Mo1 96.14(12) . 2_776
Mo4 O2 Mo1 95.72(12) . 2_776
Mo1 O3 Mo3 107.28(15) . .
Mo1 O3 Mo4 115.97(15) . 2_776
Mo3 O3 Mo4 89.45(11) . 2_776
Mo1 O5 Mo2 114.67(16) . 2_776
Mo2 O6 Mo4 114.82(17) . .
Mo3 O9 Cu1 138.4(2) . .
Mo3 O10 Mo4 116.43(17) . 2_776
Cu1 O14 Cu2 124.07(19) . .
Cu1 O14 H14 118.0 . .
Cu2 O14 H14 118.0 . .
Cu2 O15 H15A 105.5 . .
Cu2 O15 H15B 140.5 . .
H15A O15 H15B 108.5 . .
N2 C1 N3 109.8(5) . .
N2 C1 H1 125.1 . .
N3 C1 H1 125.1 . .
N1 C2 N3 109.2(5) . .
N1 C2 H2 125.4 . .
N3 C2 H2 125.4 . .
N6 C3 N7 109.3(5) . .
N6 C3 H3 125.4 . .
N7 C3 H3 125.4 . .
N5 C4 N7 108.7(4) . .
N5 C4 H4 125.6 . .
N7 C4 H4 125.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O14 1.885(3) .
Cu1 O9 1.926(4) .
Cu1 N5 1.956(4) .
Cu1 N2 1.993(4) .
Cu2 O14 1.911(4) 2_655
Cu2 O14 1.911(4) .
Cu2 N6 2.040(4) .
Cu2 N6 2.040(4) 2_655
Cu2 O15 2.631(5) .
Mo1 O4 1.707(3) .
Mo1 O5 1.754(3) .
Mo1 O3 1.869(3) .
Mo1 O2 1.942(3) .
Mo1 O1 2.207(3) .
Mo1 O2 2.484(3) 2_776
Mo2 O7 1.707(4) .
Mo2 O8 1.724(3) .
Mo2 O6 1.917(4) .
Mo2 O1 1.976(3) .
Mo2 O2 2.210(3) .
Mo2 O5 2.381(3) 2_776
Mo3 O11 1.693(4) .
Mo3 O9 1.764(4) .
Mo3 O10 1.845(3) .
Mo3 O1 2.018(3) .
Mo3 O3 2.308(3) .
Mo3 N1 2.318(4) .
Mo4 O12 1.696(4) .
Mo4 O13 1.705(4) .
Mo4 O6 1.957(3) .
Mo4 O10 1.984(4) 2_776
Mo4 O2 2.313(3) .
Mo4 O3 2.319(3) 2_776
N1 C2 1.321(6) .
N1 N2 1.384(6) .
N2 C1 1.301(6) .
N3 C1 1.344(7) .
N3 C2 1.349(7) .
N3 N4 1.402(5) .
N4 H4A 0.8600 .
N4 H4B 0.8600 .
N5 C4 1.308(6) .
N5 N6 1.376(6) .
N6 C3 1.309(6) .
N7 C4 1.346(6) .
N7 C3 1.357(6) .
N7 N8 1.413(6) .
N8 H8A 0.8600 .
N8 H8B 0.8600 .
O2 Mo1 2.484(3) 2_776
O3 Mo4 2.319(3) 2_776
O5 Mo2 2.381(3) 2_776
O10 Mo4 1.984(3) 2_776
O14 H14 0.8500 .
O15 H15A 0.8500 .
O15 H15B 0.8500 .
C1 H1 0.9300 .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 H4 0.9300 .
