#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:48:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011278.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_7011278
loop_
_publ_author_name
'Barbara Modec'
'Jurij V. Brenčič'
'Jon Zubieta'
_publ_section_title
;
 A templated synthesis of tetranuclear polyoxoalkoxymolybdates(V).
 Bromo coordinated oxomolybdenum(V) clusters: known core structure with
 new ligands. Oxidation to the Lindquist anion
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1500
_journal_page_last               1507
_journal_paper_doi               10.1039/b110062a
_journal_year                    2002
_chemical_formula_sum            'C18 H34 Br4 Mo4 N2 O12'
_chemical_formula_weight         1173.87
_chemical_name_systematic
; 
Dipyridinium tetrabromo-di-μ₂-ethoxo-diethanol-di-μ₃-
oxo-di-μ₂-oxo-tetraoxotetramolybdate(V)
;
_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                110.8365(6)
_cell_angle_beta                 104.1747(6)
_cell_angle_gamma                99.9521(6)
_cell_formula_units_Z            1
_cell_length_a                   9.21240(10)
_cell_length_b                   9.84160(10)
_cell_length_c                   10.43200(10)
_cell_measurement_reflns_used    3676
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     821.027(16)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7160
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    6.414
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.374
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0184P)²+0.9532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                3237
_reflns_number_total             3742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110062a.txt
_cod_data_source_block           1c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.9532P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.9532P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        821.026(15)
_cod_database_code               7011278
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 1.10167(3) -0.02968(3) 1.14326(3) 0.01829(8) Uani 1 d . . .
Mo2 Mo 1.14845(3) -0.18487(3) 0.90398(3) 0.01957(8) Uani 1 d . . .
Br1 Br 0.94516(4) -0.11748(4) 1.28887(4) 0.03127(10) Uani 1 d . . .
Br2 Br 1.07030(4) -0.47145(4) 0.74428(4) 0.03363(11) Uani 1 d . . .
O1 O 1.2781(3) 0.0144(3) 1.2649(2) 0.0279(5) Uani 1 d . . .
O2 O 1.3377(2) -0.1715(3) 0.9732(2) 0.0273(5) Uani 1 d . . .
O3 O 1.0441(2) -0.2464(2) 1.0227(2) 0.0211(4) Uani 1 d . . .
O4 O 1.1365(2) 0.0274(2) 0.9873(2) 0.0190(4) Uani 1 d . . .
O5 O 1.0677(2) 0.1848(2) 1.2383(2) 0.0209(4) Uani 1 d . . .
O6 O 1.2108(3) -0.1425(3) 0.7282(3) 0.0298(5) Uani 1 d . . .
H6 H 1.1751 -0.0777 0.7110 0.045 Uiso 1 calc R . .
N N 0.7528(3) -0.4374(3) 0.9154(3) 0.0332(7) Uani 1 d . . .
H0 H 0.8480 -0.3810 0.9570 0.040 Uiso 1 calc R . .
C1 C 0.7263(5) -0.5854(5) 0.8578(4) 0.0390(9) Uani 1 d . . .
H1 H 0.8098 -0.6268 0.8626 0.047 Uiso 1 calc R . .
C2 C 0.5765(5) -0.6788(4) 0.7909(4) 0.0393(9) Uani 1 d . . .
H2 H 0.5570 -0.7837 0.7501 0.047 Uiso 1 calc R . .
C3 C 0.4549(4) -0.6140(5) 0.7853(4) 0.0383(9) Uani 1 d . . .
H3 H 0.3520 -0.6751 0.7400 0.046 Uiso 1 calc R . .
C4 C 0.4870(4) -0.4581(4) 0.8474(4) 0.0352(8) Uani 1 d . . .
H4 H 0.4061 -0.4131 0.8450 0.042 Uiso 1 calc R . .
C5 C 0.6383(4) -0.3709(4) 0.9121(4) 0.0329(8) Uani 1 d . . .
H5 H 0.6619 -0.2656 0.9537 0.040 Uiso 1 calc R . .
C51 C 1.1446(4) 0.2778(4) 1.3931(3) 0.0284(7) Uani 1 d . . .
H51A H 1.1624 0.2130 1.4434 0.034 Uiso 1 calc R . .
H51B H 1.0775 0.3354 1.4311 0.034 Uiso 1 calc R . .
C52 C 1.2978(4) 0.3847(4) 1.4206(4) 0.0386(9) Uani 1 d . . .
H52A H 1.3643 0.3276 1.3835 0.058 Uiso 1 calc R . .
H52B H 1.3473 0.4446 1.5233 0.058 Uiso 1 calc R . .
H52C H 1.2798 0.4503 1.3726 0.058 Uiso 1 calc R . .
C61 C 1.3536(5) -0.1395(5) 0.6969(4) 0.0452(10) Uani 1 d . . .
H61A H 1.3872 -0.2258 0.7028 0.054 Uiso 1 calc R . .
H61B H 1.4339 -0.0479 0.7690 0.054 Uiso 1 calc R . .
C62 C 1.3348(5) -0.1441(6) 0.5491(4) 0.0508(11) Uani 1 d . . .
H62A H 1.4317 -0.1443 0.5304 0.076 Uiso 1 calc R . .
H62B H 1.3056 -0.0565 0.5442 0.076 Uiso 1 calc R . .
H62C H 1.2548 -0.2344 0.4775 0.076 Uiso 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'
Br Br -0.2901 2.4595 '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
O1 Mo1 O3 106.45(10) . . ?
O1 Mo1 O4 106.42(10) . . ?
O3 Mo1 O4 93.71(9) . . ?
O1 Mo1 O5 95.03(10) . . ?
O3 Mo1 O5 157.26(8) . . ?
O4 Mo1 O5 87.15(8) . . ?
O1 Mo1 O4 165.29(9) . 2_757 ?
O3 Mo1 O4 88.12(8) . 2_757 ?
O4 Mo1 O4 73.93(9) . 2_757 ?
O5 Mo1 O4 70.26(8) . 2_757 ?
O1 Mo1 Br1 95.86(8) . . ?
O3 Mo1 Br1 83.09(6) . . ?
O4 Mo1 Br1 157.44(6) . . ?
O5 Mo1 Br1 87.45(6) . . ?
O4 Mo1 Br1 83.64(5) 2_757 . ?
O1 Mo1 Mo2 100.54(8) . . ?
O3 Mo1 Mo2 47.61(6) . . ?
O4 Mo1 Mo2 49.20(6) . . ?
O5 Mo1 Mo2 136.18(6) . . ?
O4 Mo1 Mo2 90.75(5) 2_757 . ?
Br1 Mo1 Mo2 130.605(14) . . ?
O2 Mo2 O3 106.44(10) . . ?
O2 Mo2 O4 104.65(10) . . ?
O3 Mo2 O4 93.61(8) . . ?
O2 Mo2 O5 160.82(10) . 2_757 ?
O3 Mo2 O5 92.70(8) . 2_757 ?
O4 Mo2 O5 74.78(8) . 2_757 ?
O2 Mo2 Br2 94.28(8) . . ?
O3 Mo2 Br2 84.20(6) . . ?
O4 Mo2 Br2 160.75(6) . . ?
O5 Mo2 Br2 86.20(5) 2_757 . ?
O2 Mo2 Mo1 99.18(8) . . ?
O3 Mo2 Mo1 48.00(6) . . ?
O4 Mo2 Mo1 48.71(6) . . ?
O5 Mo2 Mo1 94.58(5) 2_757 . ?
Br2 Mo2 Mo1 132.196(14) . . ?
Mo2 O3 Mo1 84.39(8) . . ?
Mo1 O4 Mo2 82.09(8) . . ?
Mo1 O4 Mo1 106.07(9) . 2_757 ?
Mo2 O4 Mo1 106.97(9) . 2_757 ?
C51 O5 Mo1 119.81(18) . . ?
C51 O5 Mo2 128.43(18) . 2_757 ?
Mo1 O5 Mo2 107.35(9) . 2_757 ?
C1 N C5 122.8(3) . . ?
N C1 C2 120.3(3) . . ?
C1 C2 C3 118.6(3) . . ?
C4 C3 C2 119.6(3) . . ?
C5 C4 C3 119.2(3) . . ?
N C5 C4 119.5(3) . . ?
O5 C51 C52 110.6(3) . . ?
O6 C61 C62 111.5(3) . . ?
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 O1 1.672(2) . ?
Mo1 O3 1.946(2) . ?
Mo1 O4 1.977(2) . ?
Mo1 O5 2.104(2) . ?
Mo1 O4 2.290(2) 2_757 ?
Mo1 Br1 2.5902(4) . ?
Mo1 Mo2 2.6060(4) . ?
Mo2 O2 1.678(2) . ?
Mo2 O3 1.934(2) . ?
Mo2 O4 1.992(2) . ?
Mo2 O5 2.173(2) 2_757 ?
Mo2 O6 2.2007(22) . ?
Mo2 Br2 2.5722(4) . ?
O4 Mo1 2.290(2) 2_757 ?
O5 C51 1.453(4) . ?
O5 Mo2 2.173(2) 2_757 ?
O6 C61 1.429(4) . ?
N C1 1.313(5) . ?
N C5 1.334(5) . ?
C1 C2 1.367(5) . ?
C2 C3 1.381(5) . ?
C3 C4 1.380(5) . ?
C4 C5 1.360(5) . ?
C51 C52 1.503(5) . ?
C61 C62 1.492(5) . ?
