#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:30:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180397 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/66/7206690.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_7206690
loop_
_publ_author_name
'Tian, Ai-xiang'
'Liu, Xiao-jing'
'Ying, Jun'
'Zhu, Dong-xia'
'Wang, Xiu-li'
'Peng, Jun'
_publ_section_title
;
 A series of organopolymolybdate polymers linked by dual fuses:
 metal--organic moiety and organic ligand through Mo--N bonds
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              6680
_journal_paper_doi               10.1039/c1ce05649b
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C9 H14 Cu2 Mo4 N9 O14'
_chemical_formula_weight         983.1
_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                109.8290(10)
_cell_angle_beta                 96.5170(10)
_cell_angle_gamma                116.3170(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7103(9)
_cell_length_b                   11.2561(10)
_cell_length_c                   11.9413(17)
_cell_measurement_temperature    296(2)
_cell_volume                     1152.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7137
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.008
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.826
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    refo
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0335
_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)+(0.0395P)²+1.9755P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                4300
_reflns_number_total             5677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05649b.txt
_cod_data_source_block           compound-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206690
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 0.02936(4) 0.17796(4) 0.04755(3) 0.01278(9) Uani 1 1 d .
Mo2 Mo -0.31085(4) -0.09689(4) -0.06147(4) 0.01463(10) Uani 1 1 d .
Mo3 Mo -0.09763(5) 0.16726(5) 0.29174(4) 0.01687(10) Uani 1 1 d .
Mo4 Mo 0.19607(4) 0.14954(5) 0.30256(4) 0.01606(10) Uani 1 1 d .
Cu1 Cu -0.63460(8) -0.37807(8) 0.02098(6) 0.03008(17) Uani 1 1 d .
Cu2 Cu 0.38173(8) 0.52610(8) 0.62194(7) 0.03241(17) Uani 1 1 d .
O1 O -0.2692(4) 0.0581(4) 0.2904(4) 0.0309(9) Uani 1 1 d .
OW1 O -0.7085(9) -0.2549(8) 0.1656(5) 0.094(2) Uani 1 1 d .
O2 O 0.2289(4) 0.0232(4) 0.3251(3) 0.0275(8) Uani 1 1 d .
O3 O -0.0167(4) 0.2911(4) 0.0140(3) 0.0236(8) Uani 1 1 d .
O4 O 0.2778(4) 0.2998(4) 0.4452(3) 0.0304(9) Uani 1 1 d .
O5 O -0.0139(4) 0.3150(4) 0.4370(3) 0.0318(9) Uani 1 1 d .
O6 O 0.1945(3) 0.2187(4) 0.0143(3) 0.0187(7) Uani 1 1 d .
O7 O -0.4414(4) -0.2017(4) -0.0114(3) 0.0243(8) Uani 1 1 d .
O8 O -0.3442(3) -0.2326(4) -0.2282(3) 0.0191(7) Uani 1 1 d .
O9 O -0.3802(4) -0.0035(4) -0.1058(3) 0.0247(8) Uani 1 1 d .
O10 O 0.0963(3) 0.0120(3) 0.0972(3) 0.0154(7) Uani 1 1 d .
O11 O -0.1636(3) 0.0635(4) 0.0940(3) 0.0164(7) Uani 1 1 d .
O12 O -0.0086(4) 0.0598(4) 0.3051(3) 0.0207(7) Uani 1 1 d .
O13 O 0.0931(3) 0.2599(3) 0.2245(3) 0.0170(7) Uani 1 1 d .
C1 C -0.3554(6) -0.2946(6) 0.1788(5) 0.0257(11) Uani 1 1 d .
H1A H -0.3045 -0.2198 0.1558 0.031 Uiso 1 1 calc R
C2 C -0.5236(6) -0.4743(6) 0.1935(5) 0.0239(11) Uani 1 1 d .
H2A H -0.6161 -0.5497 0.1819 0.029 Uiso 1 1 calc R
C3 C -0.1382(5) -0.2592(6) 0.3231(5) 0.0253(11) Uani 1 1 d .
H3A H -0.1270 -0.2669 0.4016 0.030 Uiso 1 1 calc R
H3B H -0.0874 -0.1553 0.3424 0.030 Uiso 1 1 calc R
C4 C -0.0673(5) -0.3315(6) 0.2447(5) 0.0262(12) Uani 1 1 d .
H4A H -0.0844 -0.3295 0.1640 0.031 Uiso 1 1 calc R
H4B H 0.0378 -0.2743 0.2860 0.031 Uiso 1 1 calc R
C5 C -0.2538(6) -0.7166(6) 0.1357(5) 0.0236(11) Uani 1 1 d .
H5A H -0.3260 -0.8128 0.0800 0.028 Uiso 1 1 calc R
C6 C -0.0741(5) -0.5366(6) 0.2918(5) 0.0231(11) Uani 1 1 d .
H6A H 0.0038 -0.4791 0.3660 0.028 Uiso 1 1 calc R
C7 C 0.2964(6) 0.5971(6) 0.4234(5) 0.0271(12) Uani 1 1 d .
H7A H 0.2455 0.4994 0.3636 0.033 Uiso 1 1 calc R
C8 C 0.4212(5) 0.7866(6) 0.5973(5) 0.0223(11) Uani 1 1 d .
H8A H 0.4747 0.8502 0.6813 0.027 Uiso 1 1 calc R
C9 C 0.4355(6) 0.9744(6) 0.5251(5) 0.0265(12) Uani 1 1 d .
H9A H 0.4642 1.0408 0.6127 0.032 Uiso 1 1 calc R
H9B H 0.3550 0.9744 0.4788 0.032 Uiso 1 1 calc R
N1 N -0.5007(5) -0.3872(5) 0.1354(4) 0.0237(9) Uani 1 1 d .
N2 N -0.4017(4) -0.4422(4) 0.2692(4) 0.0194(9) Uani 1 1 d .
N3 N -0.2946(4) -0.3258(5) 0.2598(4) 0.0203(9) Uani 1 1 d .
N4 N -0.1222(4) -0.4836(4) 0.2245(4) 0.0193(9) Uani 1 1 d .
N5 N -0.2396(4) -0.6004(5) 0.1227(4) 0.0219(9) Uani 1 1 d .
N6 N -0.1522(4) -0.6819(5) 0.2387(4) 0.0194(9) Uani 1 1 d .
N7 N 0.3644(4) 0.6404(5) 0.5447(4) 0.0220(9) Uani 1 1 d .
N8 N 0.3090(5) 0.7065(5) 0.3980(4) 0.0309(11) Uani 1 1 d .
N9 N 0.3893(5) 0.8259(5) 0.5113(4) 0.0216(9) 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'
Cu Cu 0.3201 1.2651 '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
O3 Mo1 O6 104.35(17) . .
O3 Mo1 O13 105.03(16) . .
O6 Mo1 O13 101.68(14) . .
O3 Mo1 O10 103.55(15) . 2
O6 Mo1 O10 97.71(14) . 2
O13 Mo1 O10 139.97(14) . 2
O3 Mo1 O11 96.84(15) . .
O6 Mo1 O11 158.54(14) . .
O13 Mo1 O11 75.60(13) . .
O10 Mo1 O11 73.68(12) 2 .
O3 Mo1 O10 179.80(14) . .
O6 Mo1 O10 75.84(14) . .
O13 Mo1 O10 74.87(12) . .
O10 Mo1 O10 76.47(13) 2 .
O11 Mo1 O10 82.98(11) . .
O7 Mo2 O9 104.18(18) . .
O7 Mo2 O8 104.10(16) . .
O9 Mo2 O8 96.56(15) . .
O7 Mo2 O11 102.57(15) . .
O9 Mo2 O11 98.42(15) . .
O8 Mo2 O11 145.03(14) . .
O7 Mo2 O10 153.52(15) . 2
O9 Mo2 O10 102.28(15) . 2
O8 Mo2 O10 73.67(12) . 2
O11 Mo2 O10 72.34(12) . 2
O7 Mo2 O6 82.58(14) . 2
O9 Mo2 O6 172.95(15) . 2
O8 Mo2 O6 79.63(13) . 2
O11 Mo2 O6 81.83(12) . 2
O10 Mo2 O6 71.02(12) 2 2
O1 Mo3 O5 105.59(19) . .
O1 Mo3 O12 101.62(17) . .
O5 Mo3 O12 102.24(16) . .
O1 Mo3 O11 90.79(16) . .
O5 Mo3 O11 155.13(17) . .
O12 Mo3 O11 92.34(14) . .
O1 Mo3 O13 160.53(15) . .
O5 Mo3 O13 93.42(16) . .
O12 Mo3 O13 77.86(14) . .
O11 Mo3 O13 69.86(12) . .
O1 Mo3 N6 94.85(17) . 1_565
O5 Mo3 N6 82.73(17) . 1_565
O12 Mo3 N6 160.67(15) . 1_565
O11 Mo3 N6 77.25(14) . 1_565
O13 Mo3 N6 83.24(13) . 1_565
O2 Mo4 O4 105.53(18) . .
O2 Mo4 O8 101.94(16) . 2
O4 Mo4 O8 95.95(17) . 2
O2 Mo4 O12 96.46(16) . .
O4 Mo4 O12 99.43(16) . .
O8 Mo4 O12 151.86(14) 2 .
O2 Mo4 O10 92.67(15) . .
O4 Mo4 O10 160.70(16) . .
O8 Mo4 O10 73.60(12) 2 .
O12 Mo4 O10 84.53(13) . .
O2 Mo4 O13 163.19(15) . .
O4 Mo4 O13 89.75(15) . .
O8 Mo4 O13 83.00(13) 2 .
O12 Mo4 O13 73.69(13) . .
O10 Mo4 O13 73.13(11) . .
N1 Cu1 N5 166.65(18) . 2_445
N1 Cu1 OW1 97.6(2) . .
N5 Cu1 OW1 95.62(19) 2_445 .
N1 Cu1 O7 91.58(16) . .
N5 Cu1 O7 86.57(16) 2_445 .
OW1 Cu1 O7 107.0(2) . .
N7 Cu2 N2 167.76(18) . 2_556
N7 Cu2 O4 99.62(16) . .
N2 Cu2 O4 91.80(16) 2_556 .
Mo4 O4 Cu2 170.3(2) . .
Mo1 O6 Mo2 116.39(17) . 2
Mo2 O7 Cu1 169.8(2) . .
Mo2 O8 Mo4 113.53(16) . 2
Mo1 O10 Mo4 151.25(18) 2 .
Mo1 O10 Mo2 103.58(13) 2 2
Mo4 O10 Mo2 93.51(11) . 2
Mo1 O10 Mo1 103.53(13) 2 .
Mo4 O10 Mo1 97.18(12) . .
Mo2 O10 Mo1 96.49(12) 2 .
Mo2 O11 Mo3 148.36(18) . .
Mo2 O11 Mo1 106.69(14) . .
Mo3 O11 Mo1 104.54(13) . .
Mo3 O12 Mo4 114.04(17) . .
Mo1 O13 Mo3 109.65(14) . .
Mo1 O13 Mo4 113.69(15) . .
Mo3 O13 Mo4 90.47(12) . .
N3 C1 N1 109.7(5) . .
N3 C1 H1A 125.1 . .
N1 C1 H1A 125.1 . .
N2 C2 N1 113.2(5) . .
N2 C2 H2A 123.4 . .
N1 C2 H2A 123.4 . .
N3 C3 C4 112.9(4) . .
N3 C3 H3A 109.0 . .
C4 C3 H3A 109.0 . .
N3 C3 H3B 109.0 . .
C4 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
N4 C4 C3 113.5(4) . .
N4 C4 H4A 108.9 . .
C3 C4 H4A 108.9 . .
N4 C4 H4B 108.9 . .
C3 C4 H4B 108.9 . .
H4A C4 H4B 107.7 . .
N5 C5 N6 113.1(4) . .
N5 C5 H5A 123.5 . .
N6 C5 H5A 123.5 . .
N6 C6 N4 110.6(4) . .
N6 C6 H6A 124.7 . .
N4 C6 H6A 124.7 . .
N8 C7 N7 113.8(5) . .
N8 C7 H7A 123.1 . .
N7 C7 H7A 123.1 . .
N9 C8 N7 109.1(4) . .
N9 C8 H8A 125.4 . .
N7 C8 H8A 125.4 . .
N9 C9 C9 108.8(5) . 2_676
N9 C9 H9A 109.9 . .
C9 C9 H9A 109.9 2_676 .
N9 C9 H9B 109.9 . .
C9 C9 H9B 109.9 2_676 .
H9A C9 H9B 108.3 . .
C2 N1 C1 104.1(4) . .
C2 N1 Cu1 131.6(4) . .
C1 N1 Cu1 124.2(4) . .
C2 N2 N3 104.2(4) . .
C2 N2 Cu2 128.1(4) . 2_556
N3 N2 Cu2 127.5(3) . 2_556
C1 N3 N2 108.8(4) . .
C1 N3 C3 128.1(4) . .
N2 N3 C3 122.8(4) . .
C6 N4 N5 108.3(4) . .
C6 N4 C4 129.9(4) . .
N5 N4 C4 121.8(4) . .
C5 N5 N4 103.9(4) . .
C5 N5 Cu1 120.8(3) . 2_445
N4 N5 Cu1 135.2(3) . 2_445
C6 N6 C5 104.0(4) . .
C6 N6 Mo3 126.2(3) . 1_545
C5 N6 Mo3 128.9(3) . 1_545
C8 N7 C7 103.7(4) . .
C8 N7 Cu2 127.5(3) . .
C7 N7 Cu2 128.8(4) . .
C7 N8 N9 102.6(4) . .
C8 N9 N8 110.9(4) . .
C8 N9 C9 127.9(5) . .
N8 N9 C9 121.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.698(3) .
Mo1 O6 1.749(3) .
Mo1 O13 1.891(3) .
Mo1 O10 1.945(3) 2
Mo1 O11 2.150(3) .
Mo1 O10 2.490(3) .
Mo2 O7 1.706(3) .
Mo2 O9 1.708(3) .
Mo2 O8 1.928(3) .
Mo2 O11 1.931(3) .
Mo2 O10 2.220(3) 2
Mo2 O6 2.373(3) 2
Mo3 O1 1.693(4) .
Mo3 O5 1.716(3) .
Mo3 O12 1.875(3) .
Mo3 O11 2.111(3) .
Mo3 O13 2.226(3) .
Mo3 N6 2.269(4) 1_565
Mo4 O2 1.703(4) .
Mo4 O4 1.709(4) .
Mo4 O8 1.936(3) 2
Mo4 O12 1.975(3) .
Mo4 O10 2.217(3) .
Mo4 O13 2.322(3) .
Cu1 N1 1.927(4) .
Cu1 N5 1.929(4) 2_445
Cu1 OW1 2.278(5) .
Cu1 O7 2.331(4) .
Cu2 N7 1.876(4) .
Cu2 N2 1.891(4) 2_556
Cu2 O4 2.342(4) .
O6 Mo2 2.373(3) 2
O8 Mo4 1.936(3) 2
O10 Mo1 1.945(3) 2
O10 Mo2 2.220(3) 2
C1 N3 1.331(6) .
C1 N1 1.338(6) .
C1 H1A 0.9300 .
C2 N2 1.321(6) .
C2 N1 1.338(7) .
C2 H2A 0.9300 .
C3 N3 1.468(6) .
C3 C4 1.519(7) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 N4 1.460(6) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N5 1.314(7) .
C5 N6 1.358(6) .
C5 H5A 0.9300 .
C6 N6 1.319(6) .
C6 N4 1.330(6) .
C6 H6A 0.9300 .
C7 N8 1.320(7) .
C7 N7 1.353(6) .
C7 H7A 0.9300 .
C8 N9 1.315(6) .
C8 N7 1.341(6) .
C8 H8A 0.9300 .
C9 N9 1.459(6) .
C9 C9 1.522(10) 2_676
C9 H9A 0.9700 .
C9 H9B 0.9700 .
N2 N3 1.357(6) .
N2 Cu2 1.891(4) 2_556
N4 N5 1.375(5) .
N5 Cu1 1.929(4) 2_445
N6 Mo3 2.269(4) 1_545
N8 N9 1.362(6) .
