#------------------------------------------------------------------------------
#$Date: 2025-11-29 21:13:21 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303733 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/89/7718961.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_7718961
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_sum            'C28 H51 Mo2 O8'
_chemical_formula_weight         707.56
_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
_audit_update_record
;
2025-01-29 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                96.742(2)
_cell_angle_beta                 98.062(2)
_cell_angle_gamma                99.026(2)
_cell_formula_units_Z            1
_cell_length_a                   5.4859(4)
_cell_length_b                   9.5060(7)
_cell_length_c                   15.6945(11)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.82
_cell_measurement_theta_min      2.39
_cell_volume                     792.15(10)
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0263
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31924
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             367
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.034
_refine_diff_density_max         4.432
_refine_diff_density_min         -1.890
_refine_ls_extinction_coef       0.0065(10)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4841
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0454
_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)+4.3310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                4145
_reflns_number_total             4841
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01246e2.cif
_cod_data_source_block           sg39
_cod_depositor_comments
'Adding full bibliography for 7718960--7718962.cif.'
_cod_database_code               7718961
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo1 0.67897(5) 0.56215(3) 0.50937(2) 0.01378(9) Uani d . . . 1.0 . .
O O1 0.5446(4) 0.7574(2) 0.52899(16) 0.0168(4) Uani d . . . 1.0 . .
O O2 0.1640(4) 0.6284(2) 0.51097(14) 0.0114(4) Uani d . . . 1.0 . .
O O3 0.6549(5) 0.5736(3) 0.37606(16) 0.0203(5) Uani d . . . 1.0 . .
O O4 0.2761(5) 0.4402(3) 0.35537(15) 0.0200(5) Uani d . . . 1.0 . .
C C1 0.3130(6) 0.7498(3) 0.5276(2) 0.0149(5) Uani d U . . 1.0 . .
C C2 0.2065(7) 0.8827(4) 0.5505(3) 0.0273(8) Uani d U . . 1.0 . .
H H2A 0.308656 0.964198 0.530701 0.033 Uiso calc U . R 1.0 A 1
H H2B 0.035713 0.869332 0.516919 0.033 Uiso calc U . R 1.0 A 1
C C3A 0.1928(17) 0.9210(7) 0.6363(5) 0.0172(13) Uani d U P . 0.499(7) B 1
H H3A 0.251277 0.868736 0.680594 0.021 Uiso calc U P R 0.499(7) B 1
C C4A 0.0748(13) 1.0558(7) 0.6550(5) 0.0178(14) Uani d U P . 0.499(7) B 1
H H4BA 0.145744 1.130167 0.621821 0.021 Uiso calc U P R 0.499(7) B 1
H H4BB -0.10711 1.030584 0.633296 0.021 Uiso calc U P R 0.499(7) B 1
C C5A 0.1138(13) 1.1203(8) 0.7508(5) 0.0220(15) Uani d U P . 0.499(7) B 1
H H5A 0.29672 1.156948 0.769912 0.026 Uiso calc U P R 0.499(7) B 1
C C6A -0.0220(17) 1.2487(9) 0.7607(6) 0.0262(16) Uani d U P . 0.499(7) B 1
H H6AA 0.022101 1.298347 0.820609 0.039 Uiso calc U P R 0.499(7) B 1
H H6AB -0.203122 1.214656 0.747304 0.039 Uiso calc U P R 0.499(7) B 1
H H6AC 0.027928 1.315416 0.720643 0.039 Uiso calc U P R 0.499(7) B 1
C C7A 0.0313(17) 1.0119(10) 0.8090(5) 0.0297(18) Uani d U P . 0.499(7) B 1
H H7AA 0.061494 1.059043 0.869463 0.045 Uiso calc U P R 0.499(7) B 1
H H7AB 0.126575 0.933158 0.804076 0.045 Uiso calc U P R 0.499(7) B 1
H H7AC -0.147464 0.973441 0.791251 0.045 Uiso calc U P R 0.499(7) B 1
C C3B 0.3069(17) 0.9300(7) 0.6598(5) 0.0169(13) Uani d U P . 0.501(7) B 2
H H3BA 0.240085 0.851352 0.690877 0.02 Uiso calc U P R 0.501(7) B 2
H H3BB 0.491764 0.944058 0.671867 0.02 Uiso calc U P R 0.501(7) B 2
C C4B 0.2210(12) 1.0678(7) 0.6932(4) 0.0171(13) Uani d U P . 0.501(7) B 2
H H4BC 0.262151 1.140007 0.654392 0.021 Uiso calc U P R 0.501(7) B 2
H H4BD 0.318374 1.105573 0.751593 0.021 Uiso calc U P R 0.501(7) B 2
C C5B -0.0573(12) 1.0543(7) 0.6995(5) 0.0182(13) Uani d U P . 0.501(7) B 2
H H5B -0.155549 1.00444 0.642529 0.022 Uiso calc U P R 0.501(7) B 2
C C6B -0.1275(16) 1.2037(8) 0.7167(6) 0.0263(17) Uani d U P . 0.501(7) B 2
H H6BA -0.309259 1.193967 0.713149 0.039 Uiso calc U P R 0.501(7) B 2
H H6BB -0.07254 1.26198 0.673076 0.039 Uiso calc U P R 0.501(7) B 2
H H6BC -0.0455 1.250762 0.774807 0.039 Uiso calc U P R 0.501(7) B 2
C C7B -0.1271(14) 0.9655(9) 0.7702(5) 0.0249(16) Uani d U P . 0.501(7) B 2
H H7BA -0.301988 0.96698 0.776404 0.037 Uiso calc U P R 0.501(7) B 2
H H7BB -0.018853 1.006464 0.825526 0.037 Uiso calc U P R 0.501(7) B 2
H H7BC -0.105117 0.866009 0.754232 0.037 Uiso calc U P R 0.501(7) B 2
C C8 0.4582(8) 0.5071(4) 0.3265(2) 0.0240(7) Uani d U . . 1.0 . .
C C9 0.4473(12) 0.5030(5) 0.2301(3) 0.0429(13) Uani d U . . 1.0 . .
H H9A 0.525697 0.597838 0.217593 0.051 Uiso calc U . R 1.0 . .
H H9AB 0.270462 0.48329 0.201355 0.051 Uiso calc U . R 1.0 . .
C C10 0.5829(8) 0.3867(4) 0.1934(2) 0.0258(8) Uani d U . . 1.0 . .
H H10A 0.757145 0.403902 0.2245 0.031 Uiso calc U . R 1.0 . .
H H10B 0.499289 0.291566 0.203787 0.031 Uiso calc U . R 1.0 . .
C C11 0.5855(15) 0.3847(5) 0.0963(3) 0.0587(18) Uani d U . . 1.0 . .
H H11A 0.411306 0.376699 0.066613 0.07 Uiso calc U . R 1.0 . .
H H11B 0.679746 0.477964 0.087195 0.07 Uiso calc U . R 1.0 . .
C C12 0.6989(16) 0.2646(5) 0.0532(4) 0.065(2) Uani d U . . 1.0 . .
H H12 0.862574 0.279333 0.093073 0.078 Uiso calc U . R 1.0 C 3
C C13A 0.7910(17) 0.2798(10) -0.0293(5) 0.035(2) Uani d U P . 0.524(8) D 3
H H13A 0.885733 0.203047 -0.042846 0.052 Uiso calc U P R 0.524(8) D 3
H H13B 0.899907 0.373546 -0.024267 0.052 Uiso calc U P R 0.524(8) D 3
H H13C 0.64891 0.272879 -0.075975 0.052 Uiso calc U P R 0.524(8) D 3
C C14A 0.5979(15) 0.1188(9) 0.0658(5) 0.0312(18) Uani d U P . 0.524(8) D 3
H H14A 0.697859 0.051835 0.041713 0.047 Uiso calc U P R 0.524(8) D 3
H H14B 0.424251 0.09233 0.036106 0.047 Uiso calc U P R 0.524(8) D 3
H H14C 0.603489 0.114178 0.12808 0.047 Uiso calc U P R 0.524(8) D 3
C C13B 0.9392(14) 0.2957(9) 0.0688(6) 0.0261(18) Uani d U P . 0.476(8) D 4
H H13D 0.994231 0.389935 0.05169 0.039 Uiso calc U P R 0.476(8) D 4
H H13E 1.009176 0.222342 0.035536 0.039 Uiso calc U P R 0.476(8) D 4
H H13F 0.997164 0.298387 0.131024 0.039 Uiso calc U P R 0.476(8) D 4
C C14B 0.5782(15) 0.2560(9) -0.0547(5) 0.0221(16) Uani d U P . 0.476(8) D 4
H H14D 0.639735 0.180238 -0.089132 0.033 Uiso calc U P R 0.476(8) D 4
H H14E 0.630753 0.348676 -0.074161 0.033 Uiso calc U P R 0.476(8) D 4
H H14F 0.395174 0.234165 -0.062453 0.033 Uiso calc U P R 0.476(8) D 4
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Mo1 Mo1 O3 2_666 . 91.47(8) ?
Mo1 Mo1 O4 2_666 2_666 92.01(7) ?
O3 Mo1 O4 . 2_666 176.49(11) ?
Mo1 Mo1 O1 2_666 . 93.12(6) ?
O3 Mo1 O1 . . 90.67(9) ?
O4 Mo1 O1 2_666 . 88.68(9) ?
Mo1 Mo1 O2 2_666 2_666 90.19(6) ?
O3 Mo1 O2 . 2_666 88.59(9) ?
O4 Mo1 O2 2_666 2_666 91.86(9) ?
O1 Mo1 O2 . 2_666 176.63(9) ?
C1 O1 Mo1 . . 117.3(2) ?
C1 O2 Mo1 . 2_666 118.14(19) ?
C8 O3 Mo1 . . 117.7(2) ?
C8 O4 Mo1 . 2_666 116.6(2) ?
O1 C1 O2 . . 121.1(3) ?
O1 C1 C2 . . 120.5(3) ?
O2 C1 C2 . . 118.3(3) ?
C3A C2 C1 . . 117.1(4) ?
C1 C2 C3B . . 104.3(4) ?
C3A C2 H2A . . 108.0 ?
C1 C2 H2A . . 108.0 ?
C3A C2 H2B . . 108.0 ?
C1 C2 H2B . . 108.0 ?
H2A C2 H2B . . 107.3 ?
C2 C3A C4A . . 114.5(6) ?
C2 C3A H3A . . 122.7 ?
C4A C3A H3A . . 122.7 ?
C5A C4A C3A . . 114.9(6) ?
C5A C4A H4BA . . 108.5 ?
C3A C4A H4BA . . 108.5 ?
C5A C4A H4BB . . 108.5 ?
C3A C4A H4BB . . 108.5 ?
H4BA C4A H4BB . . 107.5 ?
C7A C5A C6A . . 110.7(6) ?
C7A C5A C4A . . 113.1(6) ?
C6A C5A C4A . . 109.5(6) ?
C7A C5A H5A . . 107.8 ?
C6A C5A H5A . . 107.8 ?
C4A C5A H5A . . 107.8 ?
C5A C6A H6AA . . 109.5 ?
C5A C6A H6AB . . 109.5 ?
H6AA C6A H6AB . . 109.5 ?
C5A C6A H6AC . . 109.5 ?
H6AA C6A H6AC . . 109.5 ?
H6AB C6A H6AC . . 109.5 ?
C5A C7A H7AA . . 109.5 ?
C5A C7A H7AB . . 109.5 ?
H7AA C7A H7AB . . 109.5 ?
C5A C7A H7AC . . 109.5 ?
H7AA C7A H7AC . . 109.5 ?
H7AB C7A H7AC . . 109.5 ?
C4B C3B C2 . . 110.9(6) ?
C4B C3B H3BA . . 109.5 ?
C2 C3B H3BA . . 109.5 ?
C4B C3B H3BB . . 109.5 ?
C2 C3B H3BB . . 109.5 ?
H3BA C3B H3BB . . 108.0 ?
C3B C4B C5B . . 115.9(6) ?
C3B C4B H4BC . . 108.3 ?
C5B C4B H4BC . . 108.3 ?
C3B C4B H4BD . . 108.3 ?
C5B C4B H4BD . . 108.3 ?
H4BC C4B H4BD . . 107.4 ?
C7B C5B C4B . . 111.7(6) ?
C7B C5B C6B . . 110.1(6) ?
C4B C5B C6B . . 110.3(6) ?
C7B C5B H5B . . 108.2 ?
C4B C5B H5B . . 108.2 ?
C6B C5B H5B . . 108.2 ?
C5B C6B H6BA . . 109.5 ?
C5B C6B H6BB . . 109.5 ?
H6BA C6B H6BB . . 109.5 ?
C5B C6B H6BC . . 109.5 ?
H6BA C6B H6BC . . 109.5 ?
H6BB C6B H6BC . . 109.5 ?
C5B C7B H7BA . . 109.5 ?
C5B C7B H7BB . . 109.5 ?
H7BA C7B H7BB . . 109.5 ?
C5B C7B H7BC . . 109.5 ?
H7BA C7B H7BC . . 109.5 ?
H7BB C7B H7BC . . 109.5 ?
O4 C8 O3 . . 122.2(3) ?
O4 C8 C9 . . 119.4(4) ?
O3 C8 C9 . . 118.4(4) ?
C8 C9 C10 . . 110.9(3) ?
C8 C9 H9A . . 109.5 ?
C10 C9 H9A . . 109.5 ?
C8 C9 H9AB . . 109.5 ?
C10 C9 H9AB . . 109.5 ?
H9A C9 H9AB . . 108.0 ?
C11 C10 C9 . . 112.1(4) ?
C11 C10 H10A . . 109.2 ?
C9 C10 H10A . . 109.2 ?
C11 C10 H10B . . 109.2 ?
C9 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
C12 C11 C10 . . 115.5(5) ?
C12 C11 H11A . . 108.4 ?
C10 C11 H11A . . 108.4 ?
C12 C11 H11B . . 108.4 ?
C10 C11 H11B . . 108.4 ?
H11A C11 H11B . . 107.5 ?
C14A C12 C13A . . 116.2(6) ?
C13B C12 C11 . . 110.5(6) ?
C14A C12 C11 . . 116.4(5) ?
C13A C12 C11 . . 119.6(5) ?
C13B C12 C14B . . 113.1(6) ?
C11 C12 C14B . . 102.6(6) ?
C14A C12 H12 . . 99.4 ?
C13A C12 H12 . . 99.4 ?
C11 C12 H12 . . 99.4 ?
C12 C13A H13A . . 109.5 ?
C12 C13A H13B . . 109.5 ?
H13A C13A H13B . . 109.5 ?
C12 C13A H13C . . 109.5 ?
H13A C13A H13C . . 109.5 ?
H13B C13A H13C . . 109.5 ?
C12 C14A H14A . . 109.5 ?
C12 C14A H14B . . 109.5 ?
H14A C14A H14B . . 109.5 ?
C12 C14A H14C . . 109.5 ?
H14A C14A H14C . . 109.5 ?
H14B C14A H14C . . 109.5 ?
C12 C13B H13D . . 109.5 ?
C12 C13B H13E . . 109.5 ?
H13D C13B H13E . . 109.5 ?
C12 C13B H13F . . 109.5 ?
H13D C13B H13F . . 109.5 ?
H13E C13B H13F . . 109.5 ?
C12 C14B H14D . . 109.5 ?
C12 C14B H14E . . 109.5 ?
H14D C14B H14E . . 109.5 ?
C12 C14B H14F . . 109.5 ?
H14D C14B H14F . . 109.5 ?
H14E C14B H14F . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 Mo1 2_666 2.0897(5) ?
Mo1 O3 . 2.095(2) ?
Mo1 O4 2_666 2.106(2) ?
Mo1 O1 . 2.108(2) ?
Mo1 O2 2_666 2.135(2) ?
O1 C1 . 1.258(4) ?
O2 C1 . 1.281(4) ?
O3 C8 . 1.266(5) ?
O4 C8 . 1.267(5) ?
C1 C2 . 1.500(4) ?
C2 C3A . 1.368(8) ?
C2 C3B . 1.711(9) ?
C2 H2A . 0.99 ?
C2 H2B . 0.99 ?
C3A C4A . 1.540(9) ?
C3A H3A . 0.95 ?
C4A C5A . 1.528(10) ?
C4A H4BA . 0.99 ?
C4A H4BB . 0.99 ?
C5A C7A . 1.514(11) ?
C5A C6A . 1.531(10) ?
C5A H5A . 1.0 ?
C6A H6AA . 0.98 ?
C6A H6AB . 0.98 ?
C6A H6AC . 0.98 ?
C7A H7AA . 0.98 ?
C7A H7AB . 0.98 ?
C7A H7AC . 0.98 ?
C3B C4B . 1.522(9) ?
C3B H3BA . 0.99 ?
C3B H3BB . 0.99 ?
C4B C5B . 1.530(9) ?
C4B H4BC . 0.99 ?
C4B H4BD . 0.99 ?
C5B C7B . 1.526(10) ?
C5B C6B . 1.533(9) ?
C5B H5B . 1.0 ?
C6B H6BA . 0.98 ?
C6B H6BB . 0.98 ?
C6B H6BC . 0.98 ?
C7B H7BA . 0.98 ?
C7B H7BB . 0.98 ?
C7B H7BC . 0.98 ?
C8 C9 . 1.501(5) ?
C9 C10 . 1.528(5) ?
C9 H9A . 0.99 ?
C9 H9AB . 0.99 ?
C10 C11 . 1.525(6) ?
C10 H10A . 0.99 ?
C10 H10B . 0.99 ?
C11 C12 . 1.519(7) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 C13B . 1.286(11) ?
C12 C14A . 1.457(9) ?
C12 C13A . 1.469(9) ?
C12 C14B . 1.717(10) ?
C12 H12 . 1.0 ?
C13A H13A . 0.98 ?
C13A H13B . 0.98 ?
C13A H13C . 0.98 ?
C14A H14A . 0.98 ?
C14A H14B . 0.98 ?
C14A H14C . 0.98 ?
C13B H13D . 0.98 ?
C13B H13E . 0.98 ?
C13B H13F . 0.98 ?
C14B H14D . 0.98 ?
C14B H14E . 0.98 ?
C14B H14F . 0.98 ?
