#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:13:21 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303733 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/89/7718960.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_7718960
loop_
_publ_author_name
'Gersib, Simon G.'
'Subasinghe, S. M. Supundrika'
'Mankad, Neal P.'
_publ_section_title
;
 Solubilizing dimolybdenum paddlewheel complexes for energy storage
 applications.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10546
_journal_page_last               10548
_journal_paper_doi               10.1039/d5dt01246e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C20 H36 Mo2 O8'
_chemical_formula_sum            'C20 H36 Mo2 O8'
_chemical_formula_weight         596.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-29 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                100.910(10)
_cell_angle_beta                 100.241(10)
_cell_angle_gamma                100.417(9)
_cell_formula_units_Z            1
_cell_length_a                   5.4672(15)
_cell_length_b                   9.644(3)
_cell_length_c                   12.603(4)
_cell_measurement_reflns_used    2029
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      3.07
_cell_volume                     626.1(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      115.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1569
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22504
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.587
_diffrn_reflns_theta_min         2.451
_diffrn_source                   'sealed tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1272 before and 0.1034 after correction.
The Ratio of minimum to maximum transmission is 0.6765.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       Needle
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.136
_refine_diff_density_min         -0.084
_refine_diff_density_rms         0.010
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1450P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2596
_reflns_number_total             3513
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01246e2.cif
_cod_data_source_block           sg14_1_a
_cod_depositor_comments
'Adding full bibliography for 7718960--7718962.cif.'
_cod_database_code               7718960
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C009(H009), C00B(H00e)
2.b Secondary CH2 refined with riding coordinates:
 C007(H00a,H00b), C00A(H00c,H00d)
2.c Idealised Me refined as rotating group:
 C00C(H00f,H00g,H00h), C00D(H00i,H00j,H00k), C00E(H00l,H00m,H00n), C00F(H00o,
 H00p,H00q)
;
_olex2_submission_special_instructions 'No special instructions were received'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo01 Mo 0.67718(9) 0.55998(6) 0.49679(5) 0.0357(10) Uani 1 1 d . . . . .
O002 O 0.4034(9) 0.5082(5) 0.6765(4) 0.0416(14) Uani 1 1 d . . . . .
O003 O 0.5335(9) 0.7454(5) 0.4774(4) 0.0386(14) Uani 1 1 d . . . . .
O004 O 0.7798(9) 0.6373(5) 0.6696(4) 0.0418(14) Uani 1 1 d . . . . .
O005 O 0.1540(9) 0.6194(5) 0.4853(4) 0.0416(14) Uani 1 1 d . . . . .
C006 C 0.2970(12) 0.7352(7) 0.4716(6) 0.0392(17) Uani 1 1 d . . . . .
C007 C 0.1758(13) 0.8536(7) 0.4400(6) 0.0424(18) Uani 1 1 d . . . . .
H00A H 0.267724 0.947368 0.490614 0.051 Uiso 1 1 calc R U . . .
H00B H -0.002949 0.835353 0.448603 0.051 Uiso 1 1 calc R U . . .
C008 C 0.6151(14) 0.5949(7) 0.7239(6) 0.0444(18) Uani 1 1 d . . . . .
C009 C 0.1801(14) 0.8632(8) 0.3204(7) 0.0465(19) Uani 1 1 d . . . . .
H009 H 0.361787 0.892559 0.315217 0.056 Uiso 1 1 calc R U . . .
C00A C 0.6695(17) 0.6473(9) 0.8479(7) 0.055(2) Uani 1 1 d . . . . .
H00C H 0.825422 0.725838 0.871809 0.066 Uiso 1 1 calc R U . . .
H00D H 0.703344 0.566772 0.882573 0.066 Uiso 1 1 calc R U . . .
C00B C 0.4494(17) 0.7038(9) 0.8896(7) 0.057(2) Uani 1 1 d . . . . .
H00E H 0.292310 0.624393 0.862678 0.068 Uiso 1 1 calc R U . . .
C00C C 0.0425(17) 0.9778(9) 0.2895(8) 0.058(2) Uani 1 1 d . . . . .
H00F H -0.136679 0.950437 0.293388 0.087 Uiso 1 1 calc R U . . .
H00G H 0.052762 0.985818 0.213966 0.087 Uiso 1 1 calc R U . . .
H00H H 0.122579 1.071141 0.341136 0.087 Uiso 1 1 calc R U . . .
C00D C 0.062(2) 0.7154(9) 0.2400(7) 0.062(2) Uani 1 1 d . . . . .
H00I H -0.116293 0.684720 0.243684 0.092 Uiso 1 1 calc R U . . .
H00J H 0.156691 0.643744 0.260608 0.092 Uiso 1 1 calc R U . . .
H00K H 0.071538 0.723497 0.164373 0.092 Uiso 1 1 calc R U . . .
C00E C 0.397(2) 0.8336(10) 0.8429(9) 0.067(3) Uani 1 1 d . . . . .
H00L H 0.258503 0.868216 0.871693 0.101 Uiso 1 1 calc R U . . .
H00M H 0.348009 0.804280 0.761902 0.101 Uiso 1 1 calc R U . . .
H00N H 0.551340 0.911459 0.865271 0.101 Uiso 1 1 calc R U . . .
C00F C 0.505(2) 0.7417(12) 1.0154(8) 0.080(3) Uani 1 1 d . . . . .
H00O H 0.662198 0.817098 1.043893 0.121 Uiso 1 1 calc R U . . .
H00P H 0.525964 0.655260 1.043031 0.121 Uiso 1 1 calc R U . . .
H00Q H 0.363231 0.777301 1.040280 0.121 Uiso 1 1 calc R U . . .
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
Mo01 Mo01 O002 91.29(13) 2_666 2_666 ?
Mo01 Mo01 O003 93.34(13) 2_666 . ?
Mo01 Mo01 O004 92.44(13) 2_666 . ?
Mo01 Mo01 O005 90.53(13) 2_666 2_666 ?
O002 Mo01 O003 88.24(19) 2_666 . ?
O002 Mo01 O004 176.25(17) 2_666 . ?
O002 Mo01 O005 91.30(19) 2_666 2_666 ?
O003 Mo01 O005 176.11(16) . 2_666 ?
O004 Mo01 O003 91.15(19) . . ?
O004 Mo01 O005 89.06(19) . 2_666 ?
C008 O002 Mo01 117.9(5) . 2_666 ?
C006 O003 Mo01 117.0(4) . . ?
C008 O004 Mo01 116.4(5) . . ?
C006 O005 Mo01 117.9(4) . 2_666 ?
O003 C006 O005 121.0(6) . . ?
O003 C006 C007 119.6(6) . . ?
O005 C006 C007 119.2(6) . . ?
C006 C007 H00A 109.3 . . ?
C006 C007 H00B 109.3 . . ?
C006 C007 C009 111.7(6) . . ?
H00A C007 H00B 107.9 . . ?
C009 C007 H00A 109.3 . . ?
C009 C007 H00B 109.3 . . ?
O002 C008 O004 122.0(7) . . ?
O002 C008 C00A 117.9(7) . . ?
O004 C008 C00A 120.2(7) . . ?
C007 C009 H009 108.2 . . ?
C007 C009 C00D 110.9(6) . . ?
C00C C009 C007 110.2(7) . . ?
C00C C009 H009 108.2 . . ?
C00C C009 C00D 111.0(7) . . ?
C00D C009 H009 108.2 . . ?
C008 C00A H00C 108.9 . . ?
C008 C00A H00D 108.9 . . ?
C008 C00A C00B 113.2(7) . . ?
H00C C00A H00D 107.7 . . ?
C00B C00A H00C 108.9 . . ?
C00B C00A H00D 108.9 . . ?
C00A C00B H00E 107.9 . . ?
C00E C00B C00A 111.2(7) . . ?
C00E C00B H00E 107.9 . . ?
C00F C00B C00A 110.7(8) . . ?
C00F C00B H00E 107.9 . . ?
C00F C00B C00E 111.0(8) . . ?
C009 C00C H00F 109.5 . . ?
C009 C00C H00G 109.5 . . ?
C009 C00C H00H 109.5 . . ?
H00F C00C H00G 109.5 . . ?
H00F C00C H00H 109.5 . . ?
H00G C00C H00H 109.5 . . ?
C009 C00D H00I 109.5 . . ?
C009 C00D H00J 109.5 . . ?
C009 C00D H00K 109.5 . . ?
H00I C00D H00J 109.5 . . ?
H00I C00D H00K 109.5 . . ?
H00J C00D H00K 109.5 . . ?
C00B C00E H00L 109.5 . . ?
C00B C00E H00M 109.5 . . ?
C00B C00E H00N 109.5 . . ?
H00L C00E H00M 109.5 . . ?
H00L C00E H00N 109.5 . . ?
H00M C00E H00N 109.5 . . ?
C00B C00F H00O 109.5 . . ?
C00B C00F H00P 109.5 . . ?
C00B C00F H00Q 109.5 . . ?
H00O C00F H00P 109.5 . . ?
H00O C00F H00Q 109.5 . . ?
H00P C00F H00Q 109.5 . . ?
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
Mo01 Mo01 2.0926(11) 2_666 ?
Mo01 O002 2.099(5) 2_666 ?
Mo01 O003 2.116(5) . ?
Mo01 O004 2.101(5) . ?
Mo01 O005 2.132(5) 2_666 ?
O002 C008 1.269(9) . ?
O003 C006 1.266(8) . ?
O004 C008 1.280(9) . ?
O005 C006 1.302(8) . ?
C006 C007 1.501(9) . ?
C007 H00A 0.9900 . ?
C007 H00B 0.9900 . ?
C007 C009 1.531(11) . ?
C008 C00A 1.505(11) . ?
C009 H009 1.0000 . ?
C009 C00C 1.516(11) . ?
C009 C00D 1.537(12) . ?
C00A H00C 0.9900 . ?
C00A H00D 0.9900 . ?
C00A C00B 1.541(13) . ?
C00B H00E 1.0000 . ?
C00B C00E 1.531(13) . ?
C00B C00F 1.519(13) . ?
C00C H00F 0.9800 . ?
C00C H00G 0.9800 . ?
C00C H00H 0.9800 . ?
C00D H00I 0.9800 . ?
C00D H00J 0.9800 . ?
C00D H00K 0.9800 . ?
C00E H00L 0.9800 . ?
C00E H00M 0.9800 . ?
C00E H00N 0.9800 . ?
C00F H00O 0.9800 . ?
C00F H00P 0.9800 . ?
C00F H00Q 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo01 O002 C008 O004 -2.0(9) 2_666 . . . ?
Mo01 O002 C008 C00A 178.2(5) 2_666 . . . ?
Mo01 O003 C006 O005 5.0(9) . . . . ?
Mo01 O003 C006 C007 -170.4(5) . . . . ?
Mo01 O004 C008 O002 1.6(9) . . . . ?
Mo01 O004 C008 C00A -178.6(5) . . . . ?
Mo01 O005 C006 O003 -5.5(9) 2_666 . . . ?
Mo01 O005 C006 C007 170.0(5) 2_666 . . . ?
O002 C008 C00A C00B -49.1(9) . . . . ?
O003 C006 C007 C009 66.2(9) . . . . ?
O004 C008 C00A C00B 131.1(8) . . . . ?
O005 C006 C007 C009 -109.3(7) . . . . ?
C006 C007 C009 C00C 176.7(6) . . . . ?
C006 C007 C009 C00D 53.4(8) . . . . ?
C008 C00A C00B C00E -61.4(9) . . . . ?
C008 C00A C00B C00F 174.7(7) . . . . ?
