#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:51:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179427 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/24/4332481.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_4332481
loop_
_publ_author_name
'Michailovski, Alexej'
'Rüegger, Heinz'
'Sheptyakov, Denis'
'Patzke, Greta R.'
_publ_section_title
;
 Synthesis and Characterization of Novel Fluorinated Poly(oxomolybdates)
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5641
_journal_page_last               5652
_journal_paper_doi               10.1021/ic0604359
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'F3 Mo3.11 Na1.85 O12.07, C4 H12 N, 1.925(O)'
_chemical_formula_sum            'C4 H12 F3 Mo3.11 N Na1.85 O14'
_chemical_formula_weight         695.53
_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                108.354(3)
_cell_angle_beta                 97.719(3)
_cell_angle_gamma                109.636(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1659(9)
_cell_length_b                   11.8649(13)
_cell_length_c                   11.9329(13)
_cell_measurement_reflns_used    938
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      66.364
_cell_measurement_theta_min      5.321
_cell_volume                     995.54(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15641
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         34.05
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.053
_exptl_absorpt_correction_T_max  0.8530
_exptl_absorpt_correction_T_min  0.3045
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs_new
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             667
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0349
_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)+(0.0437P)²+0.3092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5633
_reflns_number_total             7321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604359sup1.cif
_cod_data_source_block           twin_iucr
_cod_original_cell_volume        995.53(19)
_cod_database_code               4332481
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 0.73966(3) 0.76672(3) 0.73998(2) 0.02893(7) Uani 1 1 d .
Mo2 Mo 0.65566(3) 0.48520(3) 0.76423(2) 0.02746(6) Uani 1 1 d .
Mo3 Mo 0.41778(3) 0.21659(2) 0.52179(2) 0.02807(7) Uani 1 1 d .
Mo4 Mo 0.2931(4) 0.4792(3) 0.5344(3) 0.0317(3) Uani 0.1047(8) 1 d P
Na1 Na 0.22918(19) 0.50628(14) 0.56421(13) 0.0317(3) Uani 0.8953(8) 1 d P
Na2 Na 0.3637(2) 0.85609(17) 0.72430(16) 0.0531(6) Uani 0.952(6) 1 d P
F1 F 0.7527(3) 0.58096(18) 0.63514(17) 0.0345(4) Uani 1 1 d .
F2 F 0.5222(2) 0.32378(19) 0.40472(17) 0.0351(4) Uani 1 1 d .
F3 F 0.3969(2) 0.40161(18) 0.62039(17) 0.0329(4) Uani 1 1 d .
O1 O 0.6127(3) 0.6410(2) 0.80318(19) 0.0308(4) Uani 1 1 d .
O2 O 0.2126(3) 0.1931(2) 0.3997(2) 0.0327(4) Uani 1 1 d .
O3 O 0.6482(3) 0.3328(2) 0.63834(19) 0.0291(4) Uani 1 1 d .
O4 O 0.9574(3) 0.8235(3) 0.8233(2) 0.0446(6) Uani 1 1 d .
O5 O 0.6693(3) 0.8843(2) 0.8105(2) 0.0420(5) Uani 1 1 d .
O6 O 0.5453(3) 0.4231(3) 0.8567(2) 0.0429(6) Uani 1 1 d .
O7 O 0.8769(3) 0.5456(2) 0.8408(2) 0.0415(5) Uani 1 1 d .
O8 O 0.3012(3) 0.1449(2) 0.6065(2) 0.0433(6) Uani 1 1 d .
O9 O 0.4856(3) 0.1041(2) 0.4381(2) 0.0402(5) Uani 1 1 d .
O10 O 0.098(5) 0.467(3) 0.572(3) 0.0462(7) Uani 0.075(5) 1 d P
O11 O 0.9310(4) 0.3665(3) 0.5312(3) 0.0462(7) Uani 0.925(5) 1 d P
O12 O 0.1962(4) 0.6630(3) 0.7522(3) 0.0578(7) Uani 1 1 d .
O13 O 0.4322(5) 0.6964(4) 0.9731(3) 0.0654(9) Uani 1 1 d .
O14 O 0.8546(3) 0.1067(2) 0.3907(2) 0.0412(5) Uani 1 1 d .
O15 O 0.3825(6) 0.0156(5) 0.9052(3) 0.0975(14) Uani 1 1 d .
N1 N 0.9893(4) 0.2273(3) 0.8237(3) 0.0369(6) Uani 1 1 d .
C1 C 0.1054(6) 2.3620(4) 0.8427(5) 0.0580(11) Uani 1 1 d .
H11 H 0.2300 2.3750 0.8632 0.087 Uiso 1 1 calc R
H12 H 0.0837 2.4219 0.9084 0.087 Uiso 1 1 calc R
H13 H 0.0778 2.3763 0.7689 0.087 Uiso 1 1 calc R
C2 C 0.8408(6) 0.2286(5) 0.8830(5) 0.0680(13) Uani 1 1 d .
H21 H 0.7771 0.1441 0.8824 0.102 Uiso 1 1 calc R
H22 H 0.7591 0.2519 0.8387 0.102 Uiso 1 1 calc R
H23 H 0.8903 0.2908 0.9660 0.102 Uiso 1 1 calc R
C3 C 0.9085(7) 0.1471(5) 0.6912(4) 0.0626(12) Uani 1 1 d .
H31 H 0.8508 0.0576 0.6794 0.094 Uiso 1 1 calc R
H32 H 1.0015 0.1574 0.6491 0.094 Uiso 1 1 calc R
H33 H 0.8209 0.1742 0.6591 0.094 Uiso 1 1 calc R
C4 C 0.1024(7) 0.1722(5) 0.8773(5) 0.0704(14) Uani 1 1 d .
H41 H 0.0268 0.0892 0.8749 0.106 Uiso 1 1 calc R
H42 H 0.1660 0.2296 0.9607 0.106 Uiso 1 1 calc R
H43 H 0.1876 0.1623 0.8309 0.106 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
O O 0.0106 0.0060 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
O4 Mo1 O5 103.69(13) . .
O4 Mo1 O2 98.17(11) . 2_666
O5 Mo1 O2 100.85(11) . 2_666
O4 Mo1 O1 102.38(11) . .
O5 Mo1 O1 97.17(11) . .
O2 Mo1 O1 148.51(9) 2_666 .
O4 Mo1 F1 90.11(11) . .
O5 Mo1 F1 164.56(10) . .
O2 Mo1 F1 83.71(8) 2_666 .
O1 Mo1 F1 72.74(8) . .
O4 Mo1 F2 167.20(10) . 2_666
O5 Mo1 F2 86.63(10) . 2_666
O2 Mo1 F2 72.10(8) 2_666 2_666
O1 Mo1 F2 83.50(8) . 2_666
F1 Mo1 F2 80.72(7) . 2_666
O4 Mo1 Na2 140.70(10) . .
O5 Mo1 Na2 37.04(9) . .
O2 Mo1 Na2 90.98(7) 2_666 .
O1 Mo1 Na2 88.05(7) . .
F1 Mo1 Na2 128.99(6) . .
F2 Mo1 Na2 49.83(6) 2_666 .
O7 Mo2 O6 103.55(12) . .
O7 Mo2 O1 101.11(11) . .
O6 Mo2 O1 98.51(11) . .
O7 Mo2 O3 97.61(11) . .
O6 Mo2 O3 102.77(11) . .
O1 Mo2 O3 147.39(9) . .
O7 Mo2 F3 164.41(10) . .
O6 Mo2 F3 90.45(10) . .
O1 Mo2 F3 83.26(8) . .
O3 Mo2 F3 72.23(8) . .
O7 Mo2 F1 86.20(10) . .
O6 Mo2 F1 167.65(10) . .
O1 Mo2 F1 71.83(8) . .
O3 Mo2 F1 83.11(8) . .
F3 Mo2 F1 80.94(7) . .
O9 Mo3 O8 104.28(12) . .
O9 Mo3 O3 97.57(11) . .
O8 Mo3 O3 102.69(11) . .
O9 Mo3 O2 100.74(11) . .
O8 Mo3 O2 98.14(11) . .
O3 Mo3 O2 147.83(9) . .
O9 Mo3 F3 163.35(10) . .
O8 Mo3 F3 91.08(10) . .
O3 Mo3 F3 72.38(8) . .
O2 Mo3 F3 83.06(8) . .
O9 Mo3 F2 84.79(10) . .
O8 Mo3 F2 167.77(10) . .
O3 Mo3 F2 83.90(8) . .
O2 Mo3 F2 71.77(8) . .
F3 Mo3 F2 81.02(7) . .
O9 Mo3 Na2 36.79(9) . 2_666
O8 Mo3 Na2 140.70(9) . 2_666
O3 Mo3 Na2 91.09(7) . 2_666
O2 Mo3 Na2 88.02(7) . 2_666
F3 Mo3 Na2 128.22(5) . 2_666
F2 Mo3 Na2 48.01(6) . 2_666
Na1 Mo4 O10 25.7(12) . .
Na1 Mo4 F1 118.3(3) . 2_666
O10 Mo4 F1 108.8(13) . 2_666
Na1 Mo4 F3 114.4(3) . .
O10 Mo4 F3 105.9(13) . .
F1 Mo4 F3 119.70(18) 2_666 .
Na1 Mo4 F2 86.0(3) . 2_666
O10 Mo4 F2 111.7(12) . 2_666
F1 Mo4 F2 103.87(14) 2_666 2_666
F3 Mo4 F2 106.95(15) . 2_666
Mo4 Na1 O10 136(2) . .
Mo4 Na1 F2 73.7(2) . 2_666
O10 Na1 F2 151(2) . 2_666
Mo4 Na1 F3 47.9(2) . .
O10 Na1 F3 111(2) . .
F2 Na1 F3 90.99(9) 2_666 .
Mo4 Na1 F1 44.7(2) . 2_666
O10 Na1 F1 112(2) . 2_666
F2 Na1 F1 87.66(8) 2_666 2_666
F3 Na1 F1 88.46(8) . 2_666
Mo4 Na1 O11 119.4(3) . 1_455
O10 Na1 O11 17.1(19) . 1_455
F2 Na1 O11 164.47(11) 2_666 1_455
F3 Na1 O11 104.05(10) . 1_455
F1 Na1 O11 96.48(10) 2_666 1_455
Mo4 Na1 O12 146.4(3) . .
O10 Na1 O12 71.2(19) . .
F2 Na1 O12 82.76(9) 2_666 .
F3 Na1 O12 110.52(10) . .
F1 Na1 O12 158.78(11) 2_666 .
O11 Na1 O12 88.23(11) 1_455 .
Mo4 Na1 O11 121.8(3) . 2_666
O10 Na1 O11 78(2) . 2_666
F2 Na1 O11 82.85(9) 2_666 2_666
F3 Na1 O11 169.48(10) . 2_666
F1 Na1 O11 82.80(9) 2_666 2_666
O11 Na1 O11 82.83(11) 1_455 2_666
O12 Na1 O11 77.26(10) . 2_666
Mo4 Na1 Na2 121.4(2) . .
O10 Na1 Na2 103(2) . .
F2 Na1 Na2 47.78(6) 2_666 .
F3 Na1 Na2 121.44(7) . .
F1 Na1 Na2 121.53(7) 2_666 .
O11 Na1 Na2 118.64(9) 1_455 .
O12 Na1 Na2 40.44(8) . .
O11 Na1 Na2 59.67(7) 2_666 .
Mo4 Na1 Na1 132.8(3) . 2_566
O10 Na1 Na1 43(2) . 2_566
F2 Na1 Na1 120.37(8) 2_666 2_566
F3 Na1 Na1 148.38(9) . 2_566
F1 Na1 Na1 88.86(7) 2_666 2_566
O11 Na1 Na1 45.09(8) 1_455 2_566
O12 Na1 Na1 79.84(9) . 2_566
O11 Na1 Na1 37.74(6) 2_666 2_566
Na2 Na1 Na1 86.29(6) . 2_566
O15 Na2 O14 92.40(13) 1_565 2_666
O15 Na2 O12 101.29(16) 1_565 .
O14 Na2 O12 104.53(11) 2_666 .
O15 Na2 O5 89.51(13) 1_565 .
O14 Na2 O5 154.87(11) 2_666 .
O12 Na2 O5 99.64(11) . .
O15 Na2 O9 125.45(15) 1_565 2_666
O14 Na2 O9 80.12(9) 2_666 2_666
O12 Na2 O9 133.04(12) . 2_666
O5 Na2 O9 78.40(10) . 2_666
O15 Na2 F2 151.40(13) 1_565 2_666
O14 Na2 F2 116.04(10) 2_666 2_666
O12 Na2 F2 75.57(9) . 2_666
O5 Na2 F2 63.61(8) . 2_666
O9 Na2 F2 61.44(8) 2_666 2_666
O15 Na2 Mo1 113.52(12) 1_565 .
O14 Na2 Mo1 148.72(9) 2_666 .
O12 Na2 Mo1 87.90(9) . .
O5 Na2 Mo1 24.98(6) . .
O9 Na2 Mo1 70.75(7) 2_666 .
F2 Na2 Mo1 38.78(4) 2_666 .
O15 Na2 Mo3 144.25(14) 1_565 2_666
O14 Na2 Mo3 94.34(8) 2_666 2_666
O12 Na2 Mo3 110.81(10) . 2_666
O5 Na2 Mo3 70.38(7) . 2_666
O9 Na2 Mo3 23.90(6) 2_666 2_666
F2 Na2 Mo3 37.54(4) 2_666 2_666
Mo1 Na2 Mo3 54.40(3) . 2_666
O15 Na2 Na1 144.16(13) 1_565 .
O14 Na2 Na1 101.81(9) 2_666 .
O12 Na2 Na1 43.43(8) . .
O5 Na2 Na1 90.97(8) . .
O9 Na2 Na1 89.62(8) 2_666 .
F2 Na2 Na1 36.93(5) 2_666 .
Mo1 Na2 Na1 67.63(4) . .
Mo3 Na2 Na1 67.83(4) 2_666 .
Mo4 F1 Mo1 120.64(13) 2_666 .
Mo4 F1 Mo2 132.86(13) 2_666 .
Mo1 F1 Mo2 94.73(7) . .
Mo1 F1 Na1 131.72(9) . 2_666
Mo2 F1 Na1 131.13(9) . 2_666
Mo4 F2 Mo1 124.40(11) 2_666 2_666
Na1 F2 Mo1 129.74(9) 2_666 2_666
Mo4 F2 Mo3 126.99(11) 2_666 .
Na1 F2 Mo3 133.49(9) 2_666 .
Mo1 F2 Mo3 95.28(7) 2_666 .
Mo4 F2 Na2 115.59(11) 2_666 2_666
Na1 F2 Na2 95.29(8) 2_666 2_666
Mo1 F2 Na2 91.38(7) 2_666 2_666
Mo3 F2 Na2 94.44(7) . 2_666
Mo4 F3 Mo3 120.64(13) . .
Mo4 F3 Mo2 130.48(13) . .
Mo3 F3 Mo2 95.65(7) . .
Mo3 F3 Na1 132.72(9) . .
Mo2 F3 Na1 128.68(9) . .
Mo2 O1 Mo1 117.10(10) . .
Mo1 O2 Mo3 117.37(10) 2_666 .
Mo3 O3 Mo2 117.00(10) . .
Mo1 O5 Na2 117.98(13) . .
Mo3 O9 Na2 119.31(12) . 2_666
Na1 O10 O11 150(3) . 1_455
O11 O10 Mo4 132(2) 1_455 .
O10 O11 Na1 93.4(16) 1_655 2_666
Na1 O11 Na1 97.17(11) 1_655 2_666
Na2 O12 Na1 96.13(11) . .
C3 N1 C4 109.4(3) . 1_655
C3 N1 C1 110.3(3) . 1_635
C4 N1 C1 108.4(3) 1_655 1_635
C3 N1 C2 108.4(3) . .
C4 N1 C2 111.0(4) 1_655 .
C1 N1 C2 109.3(3) 1_635 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O4 1.704(2) .
Mo1 O5 1.707(2) .
Mo1 O2 1.925(2) 2_666
Mo1 O1 1.936(2) .
Mo1 F1 2.2116(18) .
Mo1 F2 2.2370(18) 2_666
Mo1 Na2 3.5701(18) .
Mo2 O7 1.699(2) .
Mo2 O6 1.705(2) .
Mo2 O1 1.922(2) .
Mo2 O3 1.929(2) .
Mo2 F3 2.2228(19) .
Mo2 F1 2.2620(18) .
Mo3 O9 1.701(2) .
Mo3 O8 1.705(2) .
Mo3 O3 1.929(2) .
Mo3 O2 1.944(2) .
Mo3 F3 2.2163(18) .
Mo3 F2 2.2373(18) .
Mo3 Na2 3.6605(19) 2_666
Mo4 Na1 0.770(3) .
Mo4 O10 1.68(3) .
Mo4 F1 1.857(3) 2_666
Mo4 F3 1.872(3) .
Mo4 F2 2.130(3) 2_666
Na1 O10 1.04(3) .
Na1 F2 2.214(2) 2_666
Na1 F3 2.299(2) .
Na1 F1 2.324(2) 2_666
Na1 O11 2.335(3) 1_455
Na1 O12 2.537(3) .
Na1 O11 2.701(3) 2_666
Na1 Na2 3.669(2) .
Na1 Na1 3.784(3) 2_566
Na2 O15 2.326(4) 1_565
Na2 O14 2.346(3) 2_666
Na2 O12 2.394(4) .
Na2 O5 2.435(3) .
Na2 O9 2.514(3) 2_666
Na2 F2 2.729(3) 2_666
Na2 Mo3 3.6605(19) 2_666
F1 Mo4 1.857(3) 2_666
F1 Na1 2.324(2) 2_666
F2 Mo4 2.130(3) 2_666
F2 Na1 2.214(2) 2_666
F2 Mo1 2.2370(18) 2_666
F2 Na2 2.729(3) 2_666
O2 Mo1 1.925(2) 2_666
O9 Na2 2.514(3) 2_666
O10 O11 1.37(3) 1_455
O11 O10 1.37(3) 1_655
O11 Na1 2.335(3) 1_655
O11 Na1 2.701(3) 2_666
O14 Na2 2.346(3) 2_666
O15 Na2 2.326(4) 1_545
N1 C3 1.480(5) .
N1 C4 1.482(5) 1_655
N1 C1 1.484(5) 1_635
N1 C2 1.486(5) .
C1 N1 1.484(5) 1_475
C4 N1 1.482(5) 1_455
