#------------------------------------------------------------------------------
#$Date: 2023-12-08 19:12:05 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288193 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/12/7011277.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_7011277
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 Cl4 Mo4 N2 O12'
_chemical_formula_weight         996.03
_chemical_name_systematic
; 
Dipyridinium tetrachloro-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                110.690(10)
_cell_angle_beta                 104.24(2)
_cell_angle_gamma                100.200(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1930(10)
_cell_length_b                   9.7236(9)
_cell_length_c                   10.441(2)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.74
_cell_measurement_theta_min      4.57
_cell_volume                     809.6(2)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       'ω/2θ 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  0.0122
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -2
_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            5069
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0191(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²+0.3121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                3387
_reflns_number_total             3882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110062a.txt
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi scan' changed to 'psi-scan'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.3121P] 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^)+(0.0383P)^2^+0.3121P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

data name '_exptl_abosrpt_process_details' was replaced with
'_exptl_absorpt_process_details' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        809.63(19)
_cod_database_code               7011277
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 1.10044(2) -0.03065(2) 1.14411(2) 0.02916(7) Uani 1 d . . .
Mo2 Mo 1.14933(2) -0.18588(2) 0.90591(2) 0.03103(7) Uani 1 d . . .
Cl1 Cl 0.94473(8) -0.11431(8) 1.27717(8) 0.04588(15) Uani 1 d . . .
Cl2 Cl 1.07470(9) -0.45762(7) 0.75125(9) 0.05164(17) Uani 1 d . . .
O1 O 1.2766(2) 0.0132(2) 1.2664(2) 0.0435(4) Uani 1 d . . .
O2 O 1.3394(2) -0.1712(2) 0.9769(2) 0.0431(4) Uani 1 d . . .
O3 O 1.04211(19) -0.25008(18) 1.02289(19) 0.0339(3) Uani 1 d . . .
O4 O 1.13802(17) 0.02885(17) 0.98969(17) 0.0293(3) Uani 1 d . . .
O5 O 1.06690(19) 0.18595(18) 1.23725(17) 0.0335(3) Uani 1 d . . .
O6 O 1.2144(2) -0.1344(2) 0.7348(2) 0.0479(5) Uani 1 d . . .
H6 H 1.1795 -0.0686 0.7172 0.072 Uiso 1 calc R . .
N N 0.7457(3) -0.4344(3) 0.9140(3) 0.0555(6) Uani 1 d . . .
H H 0.8399 -0.3739 0.9568 0.067 Uiso 1 calc R . .
C1 C 0.7252(4) -0.5828(4) 0.8563(4) 0.0617(9) Uani 1 d . . .
H1 H 0.8116 -0.6205 0.8617 0.074 Uiso 1 calc R . .
C2 C 0.5785(4) -0.6814(4) 0.7888(4) 0.0589(8) Uani 1 d . . .
H2 H 0.5629 -0.7870 0.7477 0.071 Uiso 1 calc R . .
C3 C 0.4520(4) -0.6219(4) 0.7822(3) 0.0555(8) Uani 1 d . . .
H3 H 0.3502 -0.6877 0.7365 0.067 Uiso 1 calc R . .
C4 C 0.4769(4) -0.4664(4) 0.8429(3) 0.0525(7) Uani 1 d . . .
H4 H 0.3927 -0.4254 0.8390 0.063 Uiso 1 calc R . .
C5 C 0.6268(4) -0.3728(3) 0.9092(3) 0.0536(7) Uani 1 d . . .
H5 H 0.6464 -0.2667 0.9509 0.064 Uiso 1 calc R . .
C51 C 1.1415(3) 0.2795(3) 1.3922(3) 0.0426(6) Uani 1 d . . .
H51A H 1.1575 0.2136 1.4424 0.051 Uiso 1 calc R . .
H51B H 1.0737 0.3376 1.4285 0.051 Uiso 1 calc R . .
C52 C 1.2963(4) 0.3880(4) 1.4227(3) 0.0603(8) Uani 1 d . . .
H52A H 1.3651 0.3305 1.3909 0.090 Uiso 1 calc R . .
H52B H 1.3422 0.4511 1.5252 0.090 Uiso 1 calc R . .
H52C H 1.2806 0.4521 1.3716 0.090 Uiso 1 calc R . .
C61 C 1.3498(4) -0.1408(5) 0.6935(4) 0.0681(10) Uani 1 d . . .
H61A H 1.3767 -0.2328 0.6936 0.082 Uiso 1 calc R . .
H61B H 1.4371 -0.0527 0.7643 0.082 Uiso 1 calc R . .
C62 C 1.3257(5) -0.1417(6) 0.5475(4) 0.0817(12) Uani 1 d . . .
H62A H 1.4148 -0.1585 0.5187 0.123 Uiso 1 calc R . .
H62B H 1.3136 -0.0446 0.5505 0.123 Uiso 1 calc R . .
H62C H 1.2330 -0.2224 0.4787 0.123 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 106.34(8) . . ?
O1 Mo1 O4 106.32(8) . . ?
O3 Mo1 O4 93.80(7) . . ?
O1 Mo1 O5 95.38(9) . . ?
O3 Mo1 O5 157.16(7) . . ?
O4 Mo1 O5 86.65(7) . . ?
O1 Mo1 O4 165.70(8) . 2_757 ?
O3 Mo1 O4 87.85(7) . 2_757 ?
O4 Mo1 O4 73.74(7) . 2_757 ?
O5 Mo1 O4 70.32(6) . 2_757 ?
O1 Mo1 Cl1 96.97(7) . . ?
O3 Mo1 Cl1 83.41(5) . . ?
O4 Mo1 Cl1 156.34(5) . . ?
O5 Mo1 Cl1 87.08(5) . . ?
O4 Mo1 Cl1 82.67(4) 2_757 . ?
O1 Mo1 Mo2 100.39(7) . . ?
O3 Mo1 Mo2 47.76(5) . . ?
O4 Mo1 Mo2 49.15(5) . . ?
O5 Mo1 Mo2 135.61(5) . . ?
O4 Mo1 Mo2 90.39(4) 2_757 . ?
Cl1 Mo1 Mo2 130.98(2) . . ?
O2 Mo2 O3 106.60(8) . . ?
O2 Mo2 O4 104.30(8) . . ?
O3 Mo2 O4 93.62(7) . . ?
O2 Mo2 O5 160.92(8) . 2_757 ?
O3 Mo2 O5 92.45(7) . 2_757 ?
O4 Mo2 O5 74.93(6) . 2_757 ?
O2 Mo2 Cl2 94.87(7) . . ?
O3 Mo2 Cl2 84.93(5) . . ?
O4 Mo2 Cl2 160.33(5) . . ?
O5 Mo2 Cl2 85.51(5) 2_757 . ?
O2 Mo2 Mo1 99.06(7) . . ?
O3 Mo2 Mo1 47.99(5) . . ?
O4 Mo2 Mo1 48.72(5) . . ?
O5 Mo2 Mo1 94.50(5) 2_757 . ?
Cl2 Mo2 Mo1 132.92(2) . . ?
Mo2 O3 Mo1 84.25(6) . . ?
Mo1 O4 Mo2 82.13(6) . . ?
Mo1 O4 Mo1 106.26(7) . 2_757 ?
Mo2 O4 Mo1 106.69(7) . 2_757 ?
C51 O5 Mo1 119.78(15) . . ?
C51 O5 Mo2 127.89(15) . 2_757 ?
Mo1 O5 Mo2 107.53(7) . 2_757 ?
C1 N C5 122.9(3) . . ?
N C1 C2 120.2(3) . . ?
C1 C2 C3 118.6(3) . . ?
C4 C3 C2 120.0(3) . . ?
C3 C4 C5 118.9(3) . . ?
N C5 C4 119.5(3) . . ?
O5 C51 C52 110.7(2) . . ?
O6 C61 C62 112.1(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 1.6701(18) . ?
Mo1 O3 1.9479(17) . ?
Mo1 O4 1.9789(16) . ?
Mo1 O5 2.0993(16) . ?
Mo1 O4 2.2982(16) 2_757 ?
Mo1 Cl1 2.4506(7) . ?
Mo1 Mo2 2.6083(5) . ?
Mo2 O2 1.6805(17) . ?
Mo2 O3 1.9407(17) . ?
Mo2 O4 1.9916(15) . ?
Mo2 O5 2.1731(17) 2_757 ?
Mo2 O6 2.2025(19) . ?
Mo2 Cl2 2.4203(8) . ?
O4 Mo1 2.2982(16) 2_757 ?
O5 C51 1.452(3) . ?
O5 Mo2 2.1731(17) 2_757 ?
O6 C61 1.419(3) . ?
N C1 1.309(5) . ?
N C5 1.335(4) . ?
C1 C2 1.354(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.367(5) . ?
C4 C5 1.360(4) . ?
C51 C52 1.499(4) . ?
C61 C62 1.482(5) . ?
