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#$Date: 2025-08-18 17:20:24 +0300 (Mon, 18 Aug 2025) $
#$Revision: 301776 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/51/89/1518978.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_1518978
loop_
_publ_author_name
'Malcolm H. Chisholm'
'Christopher B. Durr'
'Thomas F. Spilker'
'Philip J. Young'
_publ_section_title
;
 Molecular ordering by halide-halide interactions in dimolybdenum
 p-halobenzoates
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              300
_journal_page_last               307
_journal_volume                  424
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C28 H16 Cl4 Mo2 O8, 2(C4 H8 O)'
_chemical_formula_sum            'C36 H32 Cl4 Mo2 O10'
_chemical_formula_weight         958.29
_chemical_name_common            '[Mo2(O2C-Ph-p-Cl)4],2(THF)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                95.5760(10)
_cell_angle_beta                 99.1280(10)
_cell_angle_gamma                100.3770(10)
_cell_formula_units_Z            1
_cell_length_a                   6.74730(10)
_cell_length_b                   11.6194(2)
_cell_length_c                   12.1291(3)
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     915.74(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0288944
_diffrn_orient_matrix_UB_12      -0.0438147
_diffrn_orient_matrix_UB_13      -0.0777916
_diffrn_orient_matrix_UB_21      -0.1420469
_diffrn_orient_matrix_UB_22      -0.0339416
_diffrn_orient_matrix_UB_23      0.0101511
_diffrn_orient_matrix_UB_31      -0.0494907
_diffrn_orient_matrix_UB_32      0.0686581
_diffrn_orient_matrix_UB_33      -0.0306135
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8216
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         1.715
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0541P)²+0.0403P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.096
_reflns_number_gt                3689
_reflns_number_total             4201
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2015-424-300-307-6.cif
_cod_data_source_block           cbd044
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1518978
loop_
_space_group_symop_operation_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_disorder_assembly
_atom_site_disorder_group
C1A C -0.0450(4) 0.2307(2) 0.5110(2) 0.0300(6) Uani 1 d . .
H1A1 H -0.0097 0.1928 0.4421 0.036 Uiso 1 calc . .
H1A2 H -0.1263 0.2907 0.49 0.036 Uiso 1 calc . .
C2A C -0.1644(4) 0.1390(3) 0.5706(3) 0.0347(7) Uani 1 d . .
H2A1 H -0.2394 0.0695 0.5168 0.042 Uiso 1 calc . .
H2A2 H -0.263 0.1729 0.6096 0.042 Uiso 1 calc . .
C3A C 0.0034(4) 0.1060(3) 0.6548(3) 0.0398(8) Uani 1 d . .
H3A1 H -0.0244 0.118 0.7324 0.048 Uiso 1 calc . .
H3A2 H 0.0129 0.0225 0.6364 0.048 Uiso 1 calc . .
C4A C 0.1992(4) 0.1879(2) 0.6435(3) 0.0322(7) Uani 1 d . .
H4A1 H 0.2851 0.2174 0.7184 0.039 Uiso 1 calc . .
H4A2 H 0.279 0.1464 0.5968 0.039 Uiso 1 calc . .
O5 O 0.1352(3) 0.28301(15) 0.59047(15) 0.0224(4) Uani 1 d . .
C1 C 0.2571(4) 0.5587(2) 0.3201(2) 0.0180(5) Uani 1 d . .
C2 C 0.1312(4) 0.5885(2) 0.2190(2) 0.0182(5) Uani 1 d . .
C3 C -0.0812(4) 0.5509(2) 0.1968(2) 0.0212(5) Uani 1 d . .
H3 H -0.1468 0.507 0.2477 0.025 Uiso 1 calc . .
C4 C -0.1963(4) 0.5769(2) 0.1020(2) 0.0245(6) Uani 1 d . .
H4 H -0.3411 0.5521 0.0877 0.029 Uiso 1 calc . .
C5 C -0.0999(4) 0.6396(2) 0.0273(2) 0.0233(6) Uani 1 d . .
C6 C 0.1106(4) 0.6785(2) 0.0485(2) 0.0251(6) Uani 1 d . .
H6 H 0.1753 0.7228 -0.0024 0.03 Uiso 1 calc . .
C7 C 0.2250(4) 0.6526(2) 0.1434(2) 0.0226(5) Uani 1 d . .
H7 H 0.3695 0.6786 0.1578 0.027 Uiso 1 calc . .
C8 C 0.5408(4) 0.3102(2) 0.3604(2) 0.0180(5) Uani 1 d . .
C9 C 0.5689(4) 0.2067(2) 0.2868(2) 0.0201(5) Uani 1 d . .
C10 C 0.4260(4) 0.1009(2) 0.2707(2) 0.0265(6) Uani 1 d . .
H10 H 0.308 0.0959 0.305 0.032 Uiso 1 calc . .
C11 C 0.4553(4) 0.0036(2) 0.2053(2) 0.0296(6) Uani 1 d . .
H11 H 0.3577 -0.0684 0.1941 0.036 Uiso 1 calc . .
C12 C 0.6280(4) 0.0118(2) 0.1562(2) 0.0247(6) Uani 1 d . .
C13 C 0.7728(4) 0.1155(2) 0.1719(2) 0.0252(6) Uani 1 d . .
H13 H 0.892 0.1193 0.1388 0.03 Uiso 1 calc . .
C14 C 0.7421(4) 0.2132(2) 0.2362(2) 0.0226(5) Uani 1 d . .
H14 H 0.8392 0.2853 0.2461 0.027 Uiso 1 calc . .
Cl1 Cl -0.24607(11) 0.67023(6) -0.09456(6) 0.03335(18) Uani 1 d . .
Cl2 Cl 0.66243(12) -0.10986(6) 0.07129(6) 0.03390(18) Uani 1 d . .
Mo1 Mo 0.36841(3) 0.45004(2) 0.52158(2) 0.01604(9) Uani 1 d . .
O1 O 0.3919(2) 0.29922(14) 0.41439(14) 0.0182(4) Uani 1 d . .
O2 O 0.1716(2) 0.49394(15) 0.38522(14) 0.0178(4) Uani 1 d . .
O3 O 0.3304(2) 0.59357(15) 0.63024(14) 0.0181(4) Uani 1 d . .
O4 O 0.5506(2) 0.40062(15) 0.66111(14) 0.0177(4) Uani 1 d . .
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 0 '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'
O O 0.0106 0.006 '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
O5 C1A C2A 105.2(2) . .
O5 C1A H1A1 110.7 . .
C2A C1A H1A1 110.7 . .
O5 C1A H1A2 110.7 . .
C2A C1A H1A2 110.7 . .
H1A1 C1A H1A2 108.8 . .
C1A C2A C3A 103.1(2) . .
C1A C2A H2A1 111.1 . .
C3A C2A H2A1 111.1 . .
C1A C2A H2A2 111.1 . .
C3A C2A H2A2 111.1 . .
H2A1 C2A H2A2 109.1 . .
C4A C3A C2A 105.0(2) . .
C4A C3A H3A1 110.8 . .
C2A C3A H3A1 110.8 . .
C4A C3A H3A2 110.8 . .
C2A C3A H3A2 110.8 . .
H3A1 C3A H3A2 108.8 . .
O5 C4A C3A 105.5(2) . .
O5 C4A H4A1 110.6 . .
C3A C4A H4A1 110.6 . .
O5 C4A H4A2 110.6 . .
C3A C4A H4A2 110.6 . .
H4A1 C4A H4A2 108.8 . .
C1A O5 C4A 105.5(2) . .
O4 C1 O2 122.0(2) 2_666 .
O4 C1 C2 118.3(2) 2_666 .
O2 C1 C2 119.8(2) . .
C7 C2 C3 119.0(2) . .
C7 C2 C1 120.1(2) . .
C3 C2 C1 120.8(2) . .
C4 C3 C2 120.5(2) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C3 C4 C5 119.6(2) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
C4 C5 C6 120.8(2) . .
C4 C5 Cl1 119.5(2) . .
C6 C5 Cl1 119.7(2) . .
C7 C6 C5 119.5(2) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C6 C7 C2 120.7(2) . .
C6 C7 H7 119.7 . .
C2 C7 H7 119.7 . .
O3 C8 O1 122.0(2) 2_666 .
O3 C8 C9 118.5(2) 2_666 .
O1 C8 C9 119.4(2) . .
C10 C9 C14 119.4(2) . .
C10 C9 C8 120.2(2) . .
C14 C9 C8 120.3(2) . .
C11 C10 C9 120.3(3) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C12 C11 C10 119.4(3) . .
C12 C11 H11 120.3 . .
C10 C11 H11 120.3 . .
C11 C12 C13 121.3(3) . .
C11 C12 Cl2 119.4(2) . .
C13 C12 Cl2 119.2(2) . .
C14 C13 C12 119.2(2) . .
C14 C13 H13 120.4 . .
C12 C13 H13 120.4 . .
C13 C14 C9 120.3(3) . .
C13 C14 H14 119.8 . .
C9 C14 H14 119.8 . .
O3 Mo1 Mo1 91.87(5) . 2_666
O3 Mo1 O2 91.98(6) . .
Mo1 Mo1 O2 92.79(5) 2_666 .
O3 Mo1 O4 87.77(6) . .
Mo1 Mo1 O4 90.49(4) 2_666 .
O2 Mo1 O4 176.72(6) . .
O3 Mo1 O1 176.74(6) . .
Mo1 Mo1 O1 91.39(4) 2_666 .
O2 Mo1 O1 87.92(6) . .
O4 Mo1 O1 92.14(6) . .
C8 O1 Mo1 116.93(15) . .
C1 O2 Mo1 116.34(15) . .
C8 O3 Mo1 117.79(15) 2_666 .
C1 O4 Mo1 118.35(15) 2_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1A O5 1.423(3) .
C1A C2A 1.527(4) .
C1A H1A1 0.99 .
C1A H1A2 0.99 .
C2A C3A 1.529(4) .
C2A H2A1 0.99 .
C2A H2A2 0.99 .
C3A C4A 1.516(4) .
C3A H3A1 0.99 .
C3A H3A2 0.99 .
C4A O5 1.429(3) .
C4A H4A1 0.99 .
C4A H4A2 0.99 .
C1 O4 1.274(3) 2_666
C1 O2 1.276(3) .
C1 C2 1.484(3) .
C2 C7 1.394(4) .
C2 C3 1.395(3) .
C3 C4 1.373(4) .
C3 H3 0.95 .
C4 C5 1.385(4) .
C4 H4 0.95 .
C5 C6 1.385(4) .
C5 Cl1 1.747(3) .
C6 C7 1.371(4) .
C6 H6 0.95 .
C7 H7 0.95 .
C8 O3 1.270(3) 2_666
C8 O1 1.278(3) .
C8 C9 1.485(3) .
C9 C10 1.395(4) .
C9 C14 1.397(4) .
C10 C11 1.380(4) .
C10 H10 0.95 .
C11 C12 1.383(4) .
C11 H11 0.95 .
C12 C13 1.384(4) .
C12 Cl2 1.739(3) .
C13 C14 1.380(4) .
C13 H13 0.95 .
C14 H14 0.95 .
Mo1 O3 2.1018(17) .
Mo1 Mo1 2.1085(4) 2_666
Mo1 O2 2.1143(17) .
Mo1 O4 2.1185(16) .
Mo1 O1 2.1234(17) .
O3 C8 1.270(3) 2_666
O4 C1 1.274(3) 2_666
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139044829
