Synthesis, structure and NMR studies of trinuclear Mo3S4clusters coordinated with dithiophosphate and chiral carboxylate ligands
Gushchin, Artem L.; Hernandez-Molina, Rita; Anyushin, Alexander V.; Gallyamov, Marsel R.; Gonzalez-Platas, Javier; Moroz, Nikolay K.; Sokolov, Maxim N.; New J. Chem. 40 (2016) 7612–; doi:10.1039/C6NJ01303A

data_7055684
_publ_section_title
;
 Synthesis, structure and NMR studies of trinuclear Mo3S4clusters
 coordinated with dithiophosphate and chiral carboxylate ligands
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7612
_journal_paper_doi               10.1039/C6NJ01303A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C25 H42 Mo3 N O9 P3 S10'
_chemical_formula_sum            'C25 H42 Mo3 N O9 P3 S10'
_chemical_formula_weight         1201.92
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-15
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                112.477(5)
_cell_angle_beta                 101.227(5)
_cell_angle_gamma                103.666(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6738(5)
_cell_length_b                   13.8873(10)
_cell_length_c                   16.3146(13)
_cell_measurement_reflns_used    8756
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.42
_cell_measurement_theta_min      25.0
_cell_volume                     2251.9(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W. 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.634
_diffrn_reflns_theta_min         2.414
_diffrn_source                   Sealed-tube
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0625 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.7343.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       prism
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         11042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0490
_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/[\s^2^(Fo^2^)+2.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8483
_reflns_number_total             11042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01303a2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7055684--7055685.cif.'
_cod_database_code               7055684
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9A) = Uanis(C9)
Uanis(C5A) = Uanis(C5)
3. Others
 Sof(H19)=Sof(O10)=Sof(H10)=1-FVAR(1)
 Sof(H19A)=Sof(O9)=Sof(H9)=FVAR(1)
 Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(2)
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(2)
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(3)
 Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C19(H19A), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B), C1(H1A,H1B), C11(H11A,H11B), C5(H5A,H5B), C9(H9A,
 H9B), C5A(H5AA,H5AB), C9A(H9AA,H9AB)
4.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C13(H13), C25(H25), C14(H14), C15(H15), C21(H21),
 C24(H24), C23(H23), C22(H22)
4.d Idealised Me refined as rotating group:
 C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE,H6BF), C4(H4A,H4B,H4C), C10(H10A,H10B,H10C),
 C10(H10D,H10E,H10F), C8(H8A,H8B,H8C), C2(H2A,H2B,H2C), C12(H12A,H12B,H12C)
4.e Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'