Cycloaddition of alkynes to diimino Mo3S4cubane-type clusters: a combined experimental and theoretical approach
Pino-Chamorro, Jose A.; Laricheva, Yuliya A.; Guillamón, Eva; Fernández-Trujillo, M. Jesús; Bustelo, Emilio; Gushchin, Artem L.; Shmelev, Nikita Y.; Abramov, Pavel A.; Sokolov, Maxim N.; Llusar, Rosa; Basallote, Manuel G.; Algarra, Andrés G.; New J. Chem. 40 (2016) 7872–; doi:10.1039/C6NJ01787H

data_7055695
_publ_section_title
;
 Cycloaddition of alkynes to diimino Mo3S4cubane-type clusters: a combined
 experimental and theoretical approach
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              7872
_journal_paper_doi               10.1039/C6NJ01787H
_journal_volume                  40
_journal_year                    2016
_chemical_formula_structural     '[Mo3S4(N2C8(C4H9)2)3Cl3]Cl*5H2O'
_chemical_formula_sum            'C54 H72 Cl4 Mo3 N6 O3 S4'
_chemical_formula_weight         1411.03
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-07 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7459(2)
_cell_length_b                   24.7459(2)
_cell_length_c                   24.7459(2)
_cell_measurement_reflns_used    6700
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      61.0650
_cell_measurement_theta_min      3.5610
_cell_volume                     15153.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'SHELXLE (Sheldrick, 2011)'
_computing_publication_material  'CIFTAB-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -65.00  -10.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057   77.0000   17.0000 55

  2 omega   54.00   80.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -       84.9183   77.0000   17.0000 26

  3 omega   49.00  120.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -       84.9183   77.0000 -120.0000 71

  4 omega -122.00  -43.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057  -77.0000  120.0000 79

  5 omega -117.00  -67.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.6057 -135.0000   54.0000 50

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0027780000
_diffrn_orient_matrix_UB_12      0.0620807000
_diffrn_orient_matrix_UB_13      0.0040626000
_diffrn_orient_matrix_UB_21      0.0622167000
_diffrn_orient_matrix_UB_22      -0.0028422000
_diffrn_orient_matrix_UB_23      0.0002531000
_diffrn_orient_matrix_UB_31      0.0004461000
_diffrn_orient_matrix_UB_32      0.0041158000
_diffrn_orient_matrix_UB_33      -0.0620707000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19227
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        60.923
_diffrn_reflns_theta_max         60.923
_diffrn_reflns_theta_min         3.093
_exptl_absorpt_coefficient_mu    6.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3811
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0792P)^2^+90.6665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2602
_reflns_number_total             3811
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c6nj01787h2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7055695.cif.'
_cod_original_cell_volume        15153.4(4)
_cod_database_code               7055695
_shelx_shelxl_version_number     2014/7
_cell_oxdiff_length_a            24.7360(6)
_cell_oxdiff_length_b            24.7353(6)
_cell_oxdiff_length_c            24.7663(7)
_cell_oxdiff_angle_alpha         89.941(2)
_cell_oxdiff_angle_beta          89.990(2)
_cell_oxdiff_angle_gamma         89.963(2)
_cell_oxdiff_volume              15153.3(7)
_cell_oxdiff_measurement_reflns_used 6700
_shelx_estimated_absorpt_t_min   0.351
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              64133
_shelx_fab_checksum              28855