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_7055685
_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_absolute_configuration unk
_chemical_formula_moiety         'C26 H44 Mo3 N O9 P3 S10'
_chemical_formula_sum            'C26 H44 Mo3 N O9 P3 S10'
_chemical_formula_weight         1215.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-30 deposited with the CCDC.
2016-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.61500(14)
_cell_length_b                   15.8462(2)
_cell_length_c                   22.5039(3)
_cell_measurement_reflns_used    10079
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      73.5410
_cell_measurement_theta_min      3.9010
_cell_volume                     4498.53(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41l (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w   -111.00  46.00   1.00    1.50    --  -40.68   0.00 -30.00  157
  2  \w     29.00  93.00   1.00    1.50    --   40.68-125.00 -60.00   64
  3  \w     29.00 140.00   1.00    3.00    --  107.63 -77.00  90.00  111
  4  \w     84.00 178.00   1.00    3.00    --  107.63  41.00-141.00   94
  5  \w    145.00 177.00   1.00    3.00    --  107.63 125.00 120.00   32
  6  \w     46.00  98.00   1.00    3.00    --  107.63 -45.00-180.00   52
  7  \w     32.00  91.00   1.00    3.00    --  107.63 -41.00-114.00   59
  8  \w     41.00  75.00   1.00    3.00    --  107.63 -45.00 -60.00   34
  9  \w     98.00 126.00   1.00    3.00    --  107.63 125.00  30.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1111540000
_diffrn_orient_matrix_UB_12      -0.0066928000
_diffrn_orient_matrix_UB_13      -0.0278254000
_diffrn_orient_matrix_UB_21      -0.0258969000
_diffrn_orient_matrix_UB_22      0.0898774000
_diffrn_orient_matrix_UB_23      0.0217299000
_diffrn_orient_matrix_UB_31      0.0433619000
_diffrn_orient_matrix_UB_32      0.0363334000
_diffrn_orient_matrix_UB_33      -0.0587090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.547
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.485
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41l (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       prism
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.032(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                8375
_reflns_number_total             8805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj01303a2.cif
_cod_data_source_block           ag451_3
_cod_depositor_comments
'Adding full bibliography for 7055684--7055685.cif.'
_cod_original_cell_volume        4498.52(9)
_cod_database_code               7055685
_chemical_oxdiff_formula         'C26 H44 Mo3 N1 O9 P3 S10'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.032(11) -0.032(11)
2. 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 O(H) groups
3.a Riding coordinates:
 O9(H9)
3.b Ternary CH refined with riding coordinates:
 C19(H19)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C20(H20A,H20B)
3.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26)
3.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.796