#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:28:56 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179062 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/24/4302436.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_4302436
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 H14 Cu Mo3 N6 O11'
_chemical_formula_weight         769.66
_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                92.20(3)
_cell_angle_beta                 99.70(3)
_cell_angle_gamma                103.60(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0600(16)
_cell_length_b                   8.9000(18)
_cell_length_c                   14.400(3)
_cell_measurement_reflns_used    4614
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      3.08
_cell_volume                     986.4(4)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9801
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.591
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             742
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.780
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0323
_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)+(0.0530P)²+2.9139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                4338
_reflns_number_total             4540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900128t_si_002_01.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 '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        986.4(3)
_cod_database_code               4302436
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.26526(6) 0.01257(5) 0.65963(3) 0.01394(11) Uani 1 1 d . . .
Mo1 Mo -0.38556(4) 0.43054(3) 0.58977(2) 0.01096(9) Uani 1 1 d . . .
Mo2 Mo -0.11336(3) 0.41211(3) 0.40159(2) 0.01006(9) Uani 1 1 d . . .
Mo3 Mo 0.16912(3) 0.22626(3) 0.45581(2) 0.01033(9) Uani 1 1 d . . .
O1W O 0.4114(3) -0.0406(3) 0.5744(2) 0.0189(5) Uani 1 1 d . . .
H1C H 0.4897 -0.0729 0.6046 0.023 Uiso 1 1 calc R . .
H1B H 0.3851 -0.0271 0.5082 0.023 Uiso 1 1 d R . .
O1 O -0.1811(3) 0.4221(3) 0.28431(19) 0.0185(5) Uani 1 1 d . . .
O2 O -0.3058(3) 0.3495(3) 0.44645(19) 0.0160(5) Uani 1 1 d . . .
O3 O -0.6085(3) 0.3777(3) 0.50032(18) 0.0126(5) Uani 1 1 d . . .
O4 O -0.0654(3) 0.1987(3) 0.39951(18) 0.0139(5) Uani 1 1 d . . .
O5 O 0.1723(3) 0.1277(3) 0.5576(2) 0.0182(5) Uani 1 1 d . . .
O6 O 0.2360(4) 0.1163(3) 0.3787(2) 0.0215(6) Uani 1 1 d . . .
O7 O -0.1575(3) 0.5656(3) 0.61307(18) 0.0124(5) Uani 1 1 d . . .
O8 O -0.3600(4) 0.2529(3) 0.6178(2) 0.0230(6) Uani 1 1 d . . .
O9 O -0.0452(3) 0.6094(3) 0.45107(18) 0.0128(5) Uani 1 1 d . . .
O10 O -0.4579(4) 0.4947(4) 0.6840(2) 0.0228(6) Uani 1 1 d . . .
N1 N 0.4161(4) -0.0515(4) 0.7683(2) 0.0203(7) Uani 1 1 d . . .
N2 N 0.5573(6) -0.0676(5) 0.9137(3) 0.0344(9) Uani 1 1 d . . .
N3 N 0.5806(4) -0.1747(4) 0.8509(2) 0.0195(7) Uani 1 1 d . . .
N4 N 0.1198(4) 0.0812(4) 0.7412(2) 0.0186(6) Uani 1 1 d . . .
N5 N -0.0476(6) 0.0815(5) 0.8498(3) 0.0343(9) Uani 1 1 d . . .
N6 N -0.0412(5) 0.2075(4) 0.7994(3) 0.0244(7) Uani 1 1 d . . .
C1 C 0.4975(5) -0.1644(5) 0.7654(3) 0.0192(7) Uani 1 1 d . . .
H1A H 0.4960 -0.2263 0.7117 0.023 Uiso 1 1 calc R . .
C2 C 0.4576(6) 0.0040(6) 0.8604(3) 0.0309(10) Uani 1 1 d . . .
H2A H 0.4186 0.0858 0.8837 0.027(13) Uiso 1 1 calc R . .
C3 C 0.6822(5) -0.2856(5) 0.8837(3) 0.0238(8) Uani 1 1 d . . .
H3A H 0.7938 -0.2299 0.9201 0.029 Uiso 1 1 calc R . .
H3B H 0.7030 -0.3421 0.8296 0.029 Uiso 1 1 calc R . .
C4 C 0.5883(5) -0.3977(5) 0.9436(3) 0.0220(8) Uani 1 1 d . . .
C5 C 0.4594(6) -0.5243(6) 0.9022(3) 0.0287(9) Uani 1 1 d . . .
H5A H 0.4315 -0.5418 0.8368 0.043(17) Uiso 1 1 calc R . .
C6 C 0.6289(6) -0.3741(5) 1.0415(3) 0.0267(9) Uani 1 1 d . . .
H6A H 0.7165 -0.2892 1.0698 0.017(11) Uiso 1 1 calc R . .
C7 C 0.0551(6) 0.2048(5) 0.7347(3) 0.0227(8) Uani 1 1 d . . .
H7A H 0.0749 0.2783 0.6911 0.027 Uiso 1 1 calc R . .
C8 C 0.0519(6) 0.0097(5) 0.8127(3) 0.0305(10) Uani 1 1 d . . .
H8A H 0.0744 -0.0825 0.8334 0.035(15) Uiso 1 1 calc R . .
C9 C -0.1357(6) 0.3248(6) 0.8180(3) 0.0314(10) Uani 1 1 d . . .
H9A H -0.2571 0.2740 0.8151 0.038 Uiso 1 1 calc R . .
H9B H -0.1288 0.3967 0.7691 0.038 Uiso 1 1 calc R . .
C10 C -0.0647(6) 0.4144(5) 0.9133(3) 0.0252(9) Uani 1 1 d . . .
C11 C -0.1132(6) 0.3561(6) 0.9951(3) 0.0312(10) Uani 1 1 d . . .
H11A H -0.1897 0.2592 0.9922 0.06(2) Uiso 1 1 calc R . .
C12 C 0.0480(7) 0.5578(6) 0.9186(3) 0.0320(10) Uani 1 1 d . . .
H12A H 0.0809 0.5977 0.8638 0.06(2) 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
_geom_angle_publ_flag
O1W Cu1 N4 175.69(12) . . ?
O1W Cu1 O5 86.64(12) . . ?
N4 Cu1 O5 89.76(13) . . ?
O1W Cu1 N1 89.74(13) . . ?
N4 Cu1 N1 93.06(14) . . ?
O5 Cu1 N1 163.76(13) . . ?
O1W Cu1 O4 88.51(11) . 2_556 ?
N4 Cu1 O4 93.87(12) . 2_556 ?
O5 Cu1 O4 89.88(11) . 2_556 ?
N1 Cu1 O4 105.86(12) . 2_556 ?
O10 Mo1 O8 103.10(15) . . ?
O10 Mo1 O7 98.32(13) . . ?
O8 Mo1 O7 106.04(12) . . ?
O10 Mo1 O3 97.85(12) . . ?
O8 Mo1 O3 102.00(13) . . ?
O7 Mo1 O3 143.31(11) . . ?
O10 Mo1 O3 100.80(13) . 2_466 ?
O8 Mo1 O3 155.96(13) . 2_466 ?
O7 Mo1 O3 72.67(10) . 2_466 ?
O3 Mo1 O3 72.06(11) . 2_466 ?
O10 Mo1 O2 174.11(12) . . ?
O8 Mo1 O2 81.15(12) . . ?
O7 Mo1 O2 84.25(10) . . ?
O3 Mo1 O2 77.14(10) . . ?
O3 Mo1 O2 74.83(9) 2_466 . ?
O1 Mo2 O2 104.62(13) . . ?
O1 Mo2 O9 105.24(13) . . ?
O2 Mo2 O9 100.23(12) . . ?
O1 Mo2 O4 99.99(12) . . ?
O2 Mo2 O4 93.33(11) . . ?
O9 Mo2 O4 147.12(11) . . ?
O1 Mo2 O7 93.42(12) . 2_566 ?
O2 Mo2 O7 158.12(11) . 2_566 ?
O9 Mo2 O7 86.56(11) . 2_566 ?
O4 Mo2 O7 71.06(10) . 2_566 ?
O1 Mo2 O9 164.88(11) . 2_566 ?
O2 Mo2 O9 89.20(11) . 2_566 ?
O9 Mo2 O9 77.72(11) . 2_566 ?
O4 Mo2 O9 72.63(10) . 2_566 ?
O7 Mo2 O9 71.81(9) 2_566 2_566 ?
O1 Mo2 Mo3 116.34(10) . . ?
O2 Mo2 Mo3 115.81(9) . . ?
O9 Mo2 Mo3 112.84(8) . . ?
O4 Mo2 Mo3 35.20(7) . . ?
O7 Mo2 Mo3 43.28(7) 2_566 . ?
O9 Mo2 Mo3 50.37(6) 2_566 . ?
O6 Mo3 O5 104.83(14) . . ?
O6 Mo3 O4 100.94(13) . . ?
O5 Mo3 O4 106.96(12) . . ?
O6 Mo3 O3 98.06(12) . 1_655 ?
O5 Mo3 O3 95.64(12) . 1_655 ?
O4 Mo3 O3 145.39(11) . 1_655 ?
O6 Mo3 O7 104.43(12) . 2_566 ?
O5 Mo3 O7 149.72(12) . 2_566 ?
O4 Mo3 O7 74.72(10) . 2_566 ?
O3 Mo3 O7 72.66(10) 1_655 2_566 ?
O6 Mo3 O9 172.31(11) . 2_566 ?
O5 Mo3 O9 81.18(11) . 2_566 ?
O4 Mo3 O9 72.42(10) . 2_566 ?
O3 Mo3 O9 85.95(10) 1_655 2_566 ?
O7 Mo3 O9 70.40(9) 2_566 2_566 ?
O6 Mo3 Mo2 124.94(10) . . ?
O5 Mo3 Mo2 119.60(9) . . ?
O4 Mo3 Mo2 38.35(8) . . ?
O3 Mo3 Mo2 107.50(7) 1_655 . ?
O7 Mo3 Mo2 44.39(7) 2_566 . ?
O9 Mo3 Mo2 47.38(6) 2_566 . ?
Cu1 O1W H1C 109.5 . . ?
Cu1 O1W H1B 120.1 . . ?
H1C O1W H1B 130.4 . . ?
Mo2 O2 Mo1 130.60(14) . . ?
Mo3 O3 Mo1 147.21(14) 1_455 . ?
Mo3 O3 Mo1 104.85(11) 1_455 2_466 ?
Mo1 O3 Mo1 107.94(11) . 2_466 ?
Mo3 O4 Mo2 106.45(12) . . ?
Mo3 O4 Cu1 130.85(13) . 2_556 ?
Mo2 O4 Cu1 122.69(12) . 2_556 ?
Mo3 O5 Cu1 157.02(16) . . ?
Mo1 O7 Mo3 108.18(11) . 2_566 ?
Mo1 O7 Mo2 144.81(13) . 2_566 ?
Mo3 O7 Mo2 92.33(10) 2_566 2_566 ?
Mo2 O9 Mo2 102.28(11) . 2_566 ?
Mo2 O9 Mo3 134.63(12) . 2_566 ?
Mo2 O9 Mo3 82.25(8) 2_566 2_566 ?
C1 N1 C2 103.6(3) . . ?
C1 N1 Cu1 126.5(3) . . ?
C2 N1 Cu1 130.0(3) . . ?
C2 N2 N3 102.3(4) . . ?
C1 N3 N2 111.0(3) . . ?
C1 N3 C3 129.2(4) . . ?
N2 N3 C3 119.8(3) . . ?
C7 N4 C8 103.3(4) . . ?
C7 N4 Cu1 127.6(3) . . ?
C8 N4 Cu1 129.0(3) . . ?
C8 N5 N6 102.5(4) . . ?
C7 N6 N5 110.6(4) . . ?
C7 N6 C9 127.7(4) . . ?
N5 N6 C9 121.7(4) . . ?
N3 C1 N1 109.1(4) . . ?
N3 C1 H1A 125.5 . . ?
N1 C1 H1A 125.5 . . ?
N2 C2 N1 114.0(4) . . ?
N2 C2 H2A 123.0 . . ?
N1 C2 H2A 123.0 . . ?
N3 C3 C4 110.8(3) . . ?
N3 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C6 119.2(4) . . ?
C5 C4 C3 120.3(4) . . ?
C6 C4 C3 120.4(4) . . ?
C4 C5 C6 119.9(4) . 2_647 ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 2_647 . ?
C5 C6 C4 120.9(4) 2_647 . ?
C5 C6 H6A 119.5 2_647 . ?
C4 C6 H6A 119.5 . . ?
N6 C7 N4 109.5(4) . . ?
N6 C7 H7A 125.3 . . ?
N4 C7 H7A 125.3 . . ?
N5 C8 N4 114.1(4) . . ?
N5 C8 H8A 123.0 . . ?
N4 C8 H8A 123.0 . . ?
N6 C9 C10 112.6(3) . . ?
N6 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N6 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C12 C10 C11 119.3(4) . . ?
C12 C10 C9 119.2(4) . . ?
C11 C10 C9 121.4(5) . . ?
C10 C11 C12 120.1(5) . 2_567 ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 2_567 . ?
C10 C12 C11 120.5(5) . 2_567 ?
C10 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 2_567 . ?
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
Cu1 O1W 1.955(3) . ?
Cu1 N4 1.968(3) . ?
Cu1 O5 1.969(3) . ?
Cu1 N1 2.001(3) . ?
Cu1 O4 2.202(3) 2_556 ?
Mo1 O10 1.694(3) . ?
Mo1 O8 1.697(3) . ?
Mo1 O7 1.913(3) . ?
Mo1 O3 1.971(3) . ?
Mo1 O3 2.188(3) 2_466 ?
Mo1 O2 2.396(3) . ?
Mo2 O1 1.698(3) . ?
Mo2 O2 1.759(3) . ?
Mo2 O9 1.792(2) . ?
Mo2 O4 2.025(3) . ?
Mo2 O7 2.192(2) 2_566 ?
Mo2 O9 2.325(3) 2_566 ?
Mo2 Mo3 3.1306(9) . ?
Mo3 O6 1.688(3) . ?
Mo3 O5 1.737(3) . ?
Mo3 O4 1.881(2) . ?
Mo3 O3 1.962(3) 1_655 ?
Mo3 O7 2.148(3) 2_566 ?
Mo3 O9 2.433(3) 2_566 ?
O1W H1C 0.8200 . ?
O1W H1B 0.9601 . ?
O3 Mo3 1.962(3) 1_455 ?
O3 Mo1 2.188(3) 2_466 ?
O4 Cu1 2.202(3) 2_556 ?
O7 Mo3 2.148(3) 2_566 ?
O7 Mo2 2.192(2) 2_566 ?
O9 Mo2 2.325(3) 2_566 ?
O9 Mo3 2.433(3) 2_566 ?
N1 C1 1.325(5) . ?
N1 C2 1.356(6) . ?
N2 C2 1.308(6) . ?
N2 N3 1.355(5) . ?
N3 C1 1.316(5) . ?
N3 C3 1.467(5) . ?
N4 C7 1.323(5) . ?
N4 C8 1.356(6) . ?
N5 C8 1.302(6) . ?
N5 N6 1.355(6) . ?
N6 C7 1.312(6) . ?
N6 C9 1.471(5) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.498(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.376(6) . ?
C4 C6 1.389(6) . ?
C5 C6 1.388(6) 2_647 ?
C5 H5A 0.9300 . ?
C6 C5 1.388(6) 2_647 ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.511(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C12 1.373(7) . ?
C10 C11 1.384(6) . ?
C11 C12 1.387(7) 2_567 ?
C11 H11A 0.9300 . ?
C12 C11 1.387(7) 2_567 ?
C12 H12A 0.9300 . ?
