#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:48:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011276.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_7011276
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            'C14 H26 Cl4 Mo4 N2 O12'
_chemical_formula_weight         939.93
_chemical_name_systematic
; 
Dipyridinium tetrachloro-di-μ₂-methoxo-dimethanol-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                109.404(2)
_cell_angle_beta                 110.841(2)
_cell_angle_gamma                98.077(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0503(9)
_cell_length_b                   9.2675(9)
_cell_length_c                   9.7103(9)
_cell_measurement_temperature    150(2)
_cell_volume                     686.30(12)
_computing_cell_refinement       'SMART (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SMART (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker SMART diffractometer'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4663
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.274
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0522P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                2711
_reflns_number_total             3166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110062a.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] 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^)+(0.0522P)^2^+0.0000P] 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        686.30(11)
_cod_database_code               7011276
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 -0.51542(3) 0.34434(3) -0.66240(3) 0.01248(9) Uani 1 d . . .
Mo2 Mo -0.26294(3) 0.38688(3) -0.40138(3) 0.01299(9) Uani 1 d . . .
Cl1 Cl -0.78216(10) 0.13621(9) -0.82852(10) 0.01824(17) Uani 1 d . . .
Cl2 Cl -0.20129(10) 0.23236(10) -0.24200(10) 0.01893(17) Uani 1 d . . .
O1 O -0.4392(3) 0.2884(3) -0.7997(3) 0.0178(5) Uani 1 d . . .
O2 O -0.1271(3) 0.3435(3) -0.4785(3) 0.0181(5) Uani 1 d . . .
O3 O -0.4685(3) 0.2160(3) -0.5380(3) 0.0146(5) Uani 1 d . . .
O4 O -0.3498(3) 0.5430(3) -0.4820(3) 0.0138(4) Uani 1 d . . .
O5 O -0.6298(3) 0.4953(3) -0.7568(3) 0.0145(5) Uani 1 d . . .
O6 O -0.0565(3) 0.5913(3) -0.1983(3) 0.0176(5) Uani 1 d . . .
H6 H -0.0931 0.6678 -0.1771 0.026 Uiso 1 calc R . .
N N 0.3763(4) 0.1344(3) -0.3647(4) 0.0211(6) Uani 1 d . . .
H H 0.4410 0.1480 -0.4091 0.025 Uiso 1 calc R . .
C51 C -0.6710(4) 0.4760(4) -0.9203(4) 0.0188(7) Uani 1 d . . .
H51A H -0.6182 0.4036 -0.9664 0.028 Uiso 1 calc R . .
H51B H -0.6336 0.5780 -0.9208 0.028 Uiso 1 calc R . .
H51C H -0.7887 0.4336 -0.9829 0.028 Uiso 1 calc R . .
C61 C 0.1036(4) 0.6436(5) -0.1939(4) 0.0237(8) Uani 1 d . . .
H61A H 0.1474 0.5544 -0.2168 0.036 Uiso 1 calc R . .
H61B H 0.1772 0.7250 -0.0884 0.036 Uiso 1 calc R . .
H61C H 0.0928 0.6861 -0.2735 0.036 Uiso 1 calc R . .
C1 C 0.2388(5) 0.1797(4) -0.4058(4) 0.0261(8) Uani 1 d . . .
H1 H 0.2158 0.2264 -0.4793 0.031 Uiso 1 calc R . .
C2 C 0.1317(4) 0.1567(4) -0.3388(4) 0.0220(7) Uani 1 d . . .
H2 H 0.0359 0.1881 -0.3659 0.026 Uiso 1 calc R . .
C3 C 0.1688(4) 0.0861(4) -0.2301(4) 0.0200(7) Uani 1 d . . .
H3 H 0.0972 0.0690 -0.1843 0.024 Uiso 1 calc R . .
C4 C 0.3123(4) 0.0412(4) -0.1900(4) 0.0196(7) Uani 1 d . . .
H4 H 0.3374 -0.0071 -0.1180 0.024 Uiso 1 calc R . .
C5 C 0.4180(4) 0.0690(4) -0.2580(4) 0.0217(7) Uani 1 d . . .
H5 H 0.5167 0.0425 -0.2299 0.026 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'
Cl Cl 0.1484 0.1585 '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 107.24(10) . . ?
O1 Mo1 O4 106.20(10) . . ?
O3 Mo1 O4 93.76(9) . . ?
O1 Mo1 O5 93.79(10) . . ?
O3 Mo1 O5 158.02(9) . . ?
O4 Mo1 O5 86.26(9) . . ?
O1 Mo1 O4 164.04(10) . 2_464 ?
O3 Mo1 O4 88.50(8) . 2_464 ?
O4 Mo1 O4 74.60(9) . 2_464 ?
O5 Mo1 O4 70.28(8) . 2_464 ?
O1 Mo1 Cl1 95.37(8) . . ?
O3 Mo1 Cl1 84.59(7) . . ?
O4 Mo1 Cl1 157.81(7) . . ?
O5 Mo1 Cl1 87.18(6) . . ?
O4 Mo1 Cl1 83.23(6) 2_464 . ?
O1 Mo1 Mo2 100.64(8) . . ?
O3 Mo1 Mo2 47.78(6) . . ?
O4 Mo1 Mo2 49.24(6) . . ?
O5 Mo1 Mo2 135.41(6) . . ?
O4 Mo1 Mo2 91.86(6) 2_464 . ?
Cl1 Mo1 Mo2 132.30(2) . . ?
O2 Mo2 O3 107.42(10) . . ?
O2 Mo2 O4 105.04(10) . . ?
O3 Mo2 O4 93.73(9) . . ?
O2 Mo2 O5 161.92(10) . 2_464 ?
O3 Mo2 O5 90.60(9) . 2_464 ?
O4 Mo2 O5 74.41(9) . 2_464 ?
O2 Mo2 Cl2 94.17(8) . . ?
O3 Mo2 Cl2 85.13(7) . . ?
O4 Mo2 Cl2 160.13(7) . . ?
O5 Mo2 Cl2 85.76(6) 2_464 . ?
O2 Mo2 Mo1 99.89(8) . . ?
O3 Mo2 Mo1 48.09(6) . . ?
O4 Mo2 Mo1 48.90(6) . . ?
O5 Mo2 Mo1 93.18(6) 2_464 . ?
Cl2 Mo2 Mo1 133.22(2) . . ?
Mo2 O3 Mo1 84.13(9) . . ?
Mo1 O4 Mo2 81.86(8) . . ?
Mo1 O4 Mo1 105.40(9) . 2_464 ?
Mo2 O4 Mo1 107.86(9) . 2_464 ?
C51 O5 Mo1 122.20(19) . . ?
C51 O5 Mo2 127.81(19) . 2_464 ?
Mo1 O5 Mo2 107.01(9) . 2_464 ?
C61 O6 H6 109.5 . . ?
C5 N C1 123.2(3) . . ?
C5 N H 118.4 . . ?
C1 N H 118.4 . . ?
O5 C51 H51A 109.5 . . ?
O5 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O5 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O6 C61 H61A 109.5 . . ?
O6 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
O6 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N C1 C2 119.6(3) . . ?
N C1 H1 120.2 . . ?
C2 C1 H1 120.2 . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N C5 C4 119.0(3) . . ?
N C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
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 1.678(2) . ?
Mo1 O3 1.946(2) . ?
Mo1 O4 1.980(2) . ?
Mo1 O5 2.110(2) . ?
Mo1 O4 2.269(2) 2_464 ?
Mo1 Cl1 2.4502(8) . ?
Mo1 Mo2 2.6005(4) . ?
Mo2 O2 1.682(2) . ?
Mo2 O3 1.936(2) . ?
Mo2 O4 1.990(2) . ?
Mo2 O5 2.176(2) 2_464 ?
Mo2 O6 2.2070(23) . ?
Mo2 Cl2 2.4166(8) . ?
O4 Mo1 2.269(2) 2_464 ?
O5 C51 1.437(4) . ?
O5 Mo2 2.176(2) 2_464 ?
O6 C61 1.443(4) . ?
O6 H6 0.8200 . ?
N C5 1.337(5) . ?
N C1 1.337(5) . ?
N H 0.8600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C1 C2 1.376(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.386(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
