#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302438.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_4302438
loop_
_publ_author_name
'Bao-xia Dong'
'Qiang Xu'
_publ_section_title
;
Investigation of Flexible Organic Ligands in the Molybdate System: Delicate
Influence of a Peripheral Cluster Environment on the Isopolymolybdate
Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5861
_journal_page_last               5873
_journal_paper_doi               10.1021/ic900128t
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C12 H12 Mo3 N6 O12 Zn'
_chemical_formula_weight         785.49
_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                 104.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8900(18)
_cell_length_b                   29.900(6)
_cell_length_c                   8.1800(16)
_cell_measurement_reflns_used    4881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.11
_cell_volume                     2109.2(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω 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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20058
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.942
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0438
_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)+(0.0364P)²+18.8880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                4306
_reflns_number_total             4856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900128t_si_002_03.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        2109.2(7)
_cod_database_code               4302438
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.93764(5) 0.077966(15) 0.24364(6) 0.01430(12) Uani 1 1 d . . .
Mo2 Mo 1.08681(5) 0.043917(15) -0.04540(5) 0.01191(12) Uani 1 1 d . . .
Mo3 Mo 0.82486(5) -0.002454(17) -0.44881(6) 0.01580(12) Uani 1 1 d . . .
Zn1 Zn 0.50104(8) 0.09045(2) 0.05999(9) 0.02034(16) Uani 1 1 d . . .
O1 O 1.1204(4) -0.01728(13) -0.0340(5) 0.0155(7) Uani 1 1 d . . .
O2 O 0.9893(5) 0.04975(14) -0.2537(5) 0.0186(8) Uani 1 1 d . . .
O3 O 1.1502(5) 0.03856(13) 0.2536(5) 0.0184(8) Uani 1 1 d . . .
O4 O 0.7418(5) 0.09115(14) 0.1896(5) 0.0217(8) Uani 1 1 d . . .
O5 O 0.6902(5) 0.03720(16) -0.4312(5) 0.0255(9) Uani 1 1 d . . .
O6 O 0.9394(5) 0.03009(13) 0.4043(4) 0.0159(8) Uani 1 1 d . . .
O7 O 1.2673(5) 0.06683(14) -0.0344(5) 0.0189(8) Uani 1 1 d . . .
O8 O 0.9975(5) 0.09531(13) 0.0474(5) 0.0172(8) Uani 1 1 d . . .
O9 O 1.0203(6) 0.11922(15) 0.3775(5) 0.0268(10) Uani 1 1 d . . .
O10 O 0.7232(6) -0.03767(17) -0.5970(5) 0.0289(10) Uani 1 1 d . . .
O11 O 0.4749(6) 0.05327(19) 0.2700(6) 0.0348(12) Uani 1 1 d . . .
O12 O 0.5620(7) 0.03399(18) -0.0694(8) 0.0424(13) Uani 1 1 d . . .
N1 N 0.4310(7) 0.14884(18) 0.1596(7) 0.0277(11) Uani 1 1 d . . .
N2 N 0.4910(9) 0.1911(2) 0.1705(10) 0.0478(17) Uani 1 1 d . . .
N3 N 0.3082(7) 0.19434(18) 0.2875(7) 0.0258(11) Uani 1 1 d . . .
N4 N 0.5416(7) 0.1249(2) -0.1479(7) 0.0304(12) Uani 1 1 d . . .
N5 N 0.4427(15) 0.1423(7) -0.2791(17) 0.162(9) Uani 1 1 d . . .
N6 N 0.6574(7) 0.1440(2) -0.3400(7) 0.0278(12) Uani 1 1 d . . .
C1 C 0.3174(8) 0.1528(2) 0.2366(9) 0.0284(14) Uani 1 1 d . . .
H1A H 0.2530 0.1295 0.2528 0.034 Uiso 1 1 calc R . .
C2 C 0.4191(8) 0.2194(2) 0.2477(9) 0.0271(13) Uani 1 1 d . . .
H2A H 0.4400 0.2496 0.2696 0.032 Uiso 1 1 calc R . .
C3 C 0.2072(9) 0.2122(2) 0.3903(9) 0.0335(16) Uani 1 1 d . . .
H3B H 0.2710 0.2252 0.4926 0.040 Uiso 1 1 calc R . .
H3A H 0.1479 0.1879 0.4223 0.040 Uiso 1 1 calc R . .
C4 C 0.0976(9) 0.2472(2) 0.2975(8) 0.0295(14) Uani 1 1 d . . .
C5 C -0.0389(10) 0.2358(2) 0.1833(11) 0.0413(18) Uani 1 1 d . . .
H5A H -0.0617 0.2058 0.1586 0.07(3) Uiso 1 1 calc R . .
C6 C 0.8572(10) 0.2313(3) -0.3953(10) 0.0406(18) Uani 1 1 d . . .
H6A H 0.7661 0.2396 -0.4722 0.04(2) Uiso 1 1 calc R . .
C7 C 0.8886(8) 0.1863(2) -0.3600(8) 0.0295(14) Uani 1 1 d . . .
C8 C 1.0264(10) 0.1753(2) -0.2482(9) 0.0367(17) Uani 1 1 d . . .
H8A H 1.0508 0.1454 -0.2249 0.04(2) Uiso 1 1 calc R . .
C9 C 0.1289(9) 0.2921(2) 0.3299(10) 0.0362(16) Uani 1 1 d . . .
H9A H 0.2206 0.3005 0.4055 0.043 Uiso 1 1 calc R . .
C10 C 0.7754(9) 0.1504(3) -0.4372(9) 0.0339(16) Uani 1 1 d . . .
H10B H 0.7248 0.1586 -0.5521 0.041 Uiso 1 1 calc R . .
H10A H 0.8306 0.1226 -0.4402 0.041 Uiso 1 1 calc R . .
C11 C 0.5119(13) 0.1541(6) -0.3987(14) 0.114(7) Uani 1 1 d . . .
H11A H 0.4662 0.1669 -0.5026 0.136 Uiso 1 1 calc R . .
C12 C 0.6717(9) 0.1244(3) -0.1958(10) 0.044(2) Uani 1 1 d . . .
H12A H 0.7633 0.1116 -0.1338 0.053 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'
Zn Zn 0.2839 1.4301 '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
_geom_angle_publ_flag
O9 Mo1 O4 104.5(2) . . ?
O9 Mo1 O8 100.50(19) . . ?
O4 Mo1 O8 101.20(19) . . ?
O9 Mo1 O6 99.71(19) . . ?
O4 Mo1 O6 100.53(18) . . ?
O8 Mo1 O6 145.40(17) . . ?
O9 Mo1 O3 97.6(2) . . ?
O4 Mo1 O3 157.87(18) . . ?
O8 Mo1 O3 76.25(16) . . ?
O6 Mo1 O3 73.48(15) . . ?
O9 Mo1 O1 166.12(18) . 3_755 ?
O4 Mo1 O1 87.85(17) . 3_755 ?
O8 Mo1 O1 70.38(15) . 3_755 ?
O6 Mo1 O1 83.90(14) . 3_755 ?
O3 Mo1 O1 70.48(14) . 3_755 ?
O9 Mo1 Mo2 121.67(16) . . ?
O4 Mo1 Mo2 117.52(14) . . ?
O8 Mo1 Mo2 35.98(12) . . ?
O6 Mo1 Mo2 109.53(12) . . ?
O3 Mo1 Mo2 48.95(10) . . ?
O1 Mo1 Mo2 45.10(9) 3_755 . ?
O2 Mo2 O7 104.42(19) . . ?
O2 Mo2 O1 100.71(18) . . ?
O7 Mo2 O1 104.66(19) . . ?
O2 Mo2 O8 98.60(18) . . ?
O7 Mo2 O8 97.31(18) . . ?
O1 Mo2 O8 145.92(16) . . ?
O2 Mo2 O1 94.08(17) . 3_755 ?
O7 Mo2 O1 160.72(16) . 3_755 ?
O1 Mo2 O1 76.60(17) . 3_755 ?
O8 Mo2 O1 74.24(15) . 3_755 ?
O2 Mo2 O3 163.89(18) . . ?
O7 Mo2 O3 89.33(17) . . ?
O1 Mo2 O3 83.50(15) . . ?
O8 Mo2 O3 70.88(15) . . ?
O1 Mo2 O3 71.60(14) 3_755 . ?
O2 Mo2 Mo1 120.51(14) . . ?
O7 Mo2 Mo1 112.85(13) . . ?
O1 Mo2 Mo1 111.95(12) . . ?
O8 Mo2 Mo1 34.24(11) . . ?
O1 Mo2 Mo1 51.08(10) 3_755 . ?
O3 Mo2 Mo1 44.53(10) . . ?
O10 Mo3 O5 103.2(2) . . ?
O10 Mo3 O3 100.5(2) . 3_755 ?
O5 Mo3 O3 105.32(19) . 3_755 ?
O10 Mo3 O6 97.66(19) . 1_554 ?
O5 Mo3 O6 100.43(19) . 1_554 ?
O3 Mo3 O6 143.96(17) 3_755 1_554 ?
O10 Mo3 O6 101.9(2) . 3_755 ?
O5 Mo3 O6 154.43(19) . 3_755 ?
O3 Mo3 O6 74.61(16) 3_755 3_755 ?
O6 Mo3 O6 71.31(17) 1_554 3_755 ?
O10 Mo3 O2 174.17(18) . . ?
O5 Mo3 O2 79.81(19) . . ?
O3 Mo3 O2 83.38(16) 3_755 . ?
O6 Mo3 O2 76.79(14) 1_554 . ?
O6 Mo3 O2 74.76(14) 3_755 . ?
N1 Zn1 N4 91.9(2) . . ?
N1 Zn1 O11 91.2(2) . . ?
N4 Zn1 O11 175.9(2) . . ?
N1 Zn1 O12 173.5(2) . . ?
N4 Zn1 O12 82.6(2) . . ?
O11 Zn1 O12 94.5(2) . . ?
N1 Zn1 O4 98.9(2) . . ?
N4 Zn1 O4 92.8(2) . . ?
O11 Zn1 O4 84.06(18) . . ?
O12 Zn1 O4 84.8(2) . . ?
N1 Zn1 O7 93.5(2) . 1_455 ?
N4 Zn1 O7 102.2(2) . 1_455 ?
O11 Zn1 O7 80.29(17) . 1_455 ?
O12 Zn1 O7 84.36(19) . 1_455 ?
O4 Zn1 O7 160.18(16) . 1_455 ?
Mo2 O1 Mo2 103.40(17) . 3_755 ?
Mo2 O1 Mo1 133.52(18) . 3_755 ?
Mo2 O1 Mo1 83.81(13) 3_755 3_755 ?
Mo2 O2 Mo3 131.1(2) . . ?
Mo3 O3 Mo1 104.98(18) 3_755 . ?
Mo3 O3 Mo2 148.7(2) 3_755 . ?
Mo1 O3 Mo2 86.52(14) . . ?
Mo1 O4 Zn1 160.5(3) . . ?
Mo1 O6 Mo3 147.3(2) . 1_556 ?
Mo1 O6 Mo3 103.90(17) . 3_755 ?
Mo3 O6 Mo3 108.69(17) 1_556 3_755 ?
Mo2 O7 Zn1 162.3(2) . 1_655 ?
Mo1 O8 Mo2 109.78(19) . . ?
C1 N1 N2 102.6(6) . . ?
C1 N1 Zn1 126.7(5) . . ?
N2 N1 Zn1 130.7(5) . . ?
C2 N2 N1 113.6(7) . . ?
C1 N3 C2 110.1(6) . . ?
C1 N3 C3 128.0(6) . . ?
C2 N3 C3 121.5(5) . . ?
C12 N4 N5 102.9(7) . . ?
C12 N4 Zn1 125.3(5) . . ?
N5 N4 Zn1 130.1(7) . . ?
N4 N5 C11 111.7(10) . . ?
C12 N6 C11 108.0(7) . . ?
C12 N6 C10 128.6(6) . . ?
C11 N6 C10 123.0(6) . . ?
N1 C1 N3 110.4(6) . . ?
N1 C1 H1A 124.8 . . ?
N3 C1 H1A 124.8 . . ?
N2 C2 N3 103.3(6) . . ?
N2 C2 H2A 128.3 . . ?
N3 C2 H2A 128.3 . . ?
N3 C3 C4 112.0(6) . . ?
N3 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
N3 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
H3B C3 H3A 107.9 . . ?
C9 C4 C5 118.1(7) . . ?
C9 C4 C3 120.2(7) . . ?
C5 C4 C3 121.6(7) . . ?
C4 C5 C6 120.8(7) . 4_466 ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 4_466 . ?
C7 C6 C5 120.6(7) . 4_665 ?
C7 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 4_665 . ?
C8 C7 C6 118.0(7) . . ?
C8 C7 C10 120.4(7) . . ?
C6 C7 C10 121.6(7) . . ?
C7 C8 C9 121.3(7) . 4_665 ?
C7 C8 H8A 119.4 . . ?
C9 C8 H8A 119.4 4_665 . ?
C8 C9 C4 121.1(7) 4_466 . ?
C8 C9 H9A 119.4 4_466 . ?
C4 C9 H9A 119.4 . . ?
N6 C10 C7 111.0(6) . . ?
N6 C10 H10B 109.4 . . ?
C7 C10 H10B 109.4 . . ?
N6 C10 H10A 109.4 . . ?
C7 C10 H10A 109.4 . . ?
H10B C10 H10A 108.0 . . ?
N6 C11 N5 105.3(8) . . ?
N6 C11 H11A 127.3 . . ?
N5 C11 H11A 127.3 . . ?
N6 C12 N4 111.7(7) . . ?
N6 C12 H12A 124.2 . . ?
N4 C12 H12A 124.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O9 1.694(4) . ?
Mo1 O4 1.735(4) . ?
Mo1 O8 1.882(4) . ?
Mo1 O6 1.940(4) . ?
Mo1 O3 2.212(4) . ?
Mo1 O1 2.464(4) 3_755 ?
Mo1 Mo2 3.1478(9) . ?
Mo2 O2 1.722(4) . ?
Mo2 O7 1.727(4) . ?
Mo2 O1 1.853(4) . ?
Mo2 O8 1.965(4) . ?
Mo2 O1 2.243(4) 3_755 ?
Mo2 O3 2.378(4) . ?
Mo3 O10 1.692(4) . ?
Mo3 O5 1.715(4) . ?
Mo3 O3 1.895(4) 3_755 ?
Mo3 O6 2.006(4) 1_554 ?
Mo3 O6 2.199(4) 3_755 ?
Mo3 O2 2.447(4) . ?
Zn1 N1 2.085(6) . ?
Zn1 N4 2.093(6) . ?
Zn1 O11 2.106(5) . ?
Zn1 O12 2.131(5) . ?
Zn1 O4 2.145(4) . ?
Zn1 O7 2.153(4) 1_455 ?
O1 Mo2 2.243(4) 3_755 ?
O1 Mo1 2.464(4) 3_755 ?
O3 Mo3 1.895(4) 3_755 ?
O6 Mo3 2.006(4) 1_556 ?
O6 Mo3 2.199(4) 3_755 ?
O7 Zn1 2.153(4) 1_655 ?
N1 C1 1.319(9) . ?
N1 N2 1.367(9) . ?
N2 C2 1.310(10) . ?
N3 C1 1.319(8) . ?
N3 C2 1.340(8) . ?
N3 C3 1.471(9) . ?
N4 C12 1.308(9) . ?
N4 N5 1.318(12) . ?
N5 C11 1.324(14) . ?
N6 C12 1.296(9) . ?
N6 C11 1.301(11) . ?
N6 C10 1.474(8) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.504(10) . ?
C3 H3B 0.9700 . ?
C3 H3A 0.9700 . ?
C4 C9 1.382(10) . ?
C4 C5 1.382(11) . ?
C5 C6 1.394(11) 4_466 ?
C5 H5A 0.9300 . ?
C6 C7 1.391(10) . ?
C6 C5 1.394(11) 4_665 ?
C6 H6A 0.9300 . ?
C7 C8 1.379(10) . ?
C7 C10 1.501(10) . ?
C8 C9 1.380(10) 4_665 ?
C8 H8A 0.9300 . ?
C9 C8 1.380(10) 4_466 ?
C9 H9A 0.9300 . ?
C10 H10B 0.9700 . ?
C10 H10A 0.9700 . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
