Electronic tuning of Mo2(thioamidate)4 complexes through π-system substituents and cis/trans isomerism.
Dolinar, Brian S.; Berry, John F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 6165–6176; doi:10.1039/c4dt00297k

data_7029518
_publ_section_title
;
 Electronic tuning of Mo2(thioamidate)4 complexes through \p-system
 substituents and cis/trans isomerism.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6165
_journal_page_last               6176
_journal_paper_doi               10.1039/c4dt00297k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C16 H16 Mo2 N4 S8, C H2 Cl2'
_chemical_formula_sum            'C17 H18 Cl2 Mo2 N4 S8'
_chemical_formula_weight         797.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-18
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.322(6)
_cell_length_b                   10.791(4)
_cell_length_c                   16.081(7)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.29
_cell_volume                     2730.1(19)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ \w and 0.5\ \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35363
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.942
_diffrn_reflns_theta_min         1.294
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7348
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.7348.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+26.4048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4343
_reflns_number_total             5323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00297k2.cif
_cod_data_source_block           2_CH2Cl2_100K
_cod_original_cell_volume        2730.3(19)
_cod_database_code               7029518
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H15A(0.039) H15B(0.039) H11A(0.024) H11B(0.024) H14A(0.042)
 H14B(0.042) H10A(0.025) H10B(0.025) H2A(0.028) H2B(0.028) H6A(0.03) H6B(0.03)
 H7A(0.031) H7B(0.031) H3A(0.027) H3B(0.027) H1SA(0.036) H1SB(0.036)
 Fixed X: H15A(0.5248) H15B(0.4729) H11A(-0.0675) H11B(-0.0145) H14A(0.3958)
 H14B(0.4426) H10A(0.0827) H10B(0.0315) H2A(0.3271) H2B(0.3887) H6A(0.0965)
 H6B(0.0426) H7A(0.1451) H7B(0.1937) H3A(0.2914) H3B(0.2323) H1SA(0.323)
 H1SB(0.2673)
 Fixed Y: H15A(0.2294) H15B(0.2863) H11A(0.3854) H11B(0.3026) H14A(0.1114)
 H14B(0.0593) H10A(0.4538) H10B(0.5344) H2A(0.0637) H2B(0.0008) H6A(0.4675)
 H6B(0.545) H7A(0.6871) H7B(0.618) H3A(-0.1455) H3B(-0.0876) H1SA(0.6932)
 H1SB(0.8167)
 Fixed Z: H15A(0.089) H15B(-0.0024) H11A(-0.1001) H11B(-0.151) H14A(-0.0289)
 H14B(0.0659) H10A(-0.1341) H10B(-0.0798) H2A(0.4383) H2B(0.3868) H6A(0.3838)
 H6B(0.3017) H7A(0.3205) H7B(0.4086) H3A(0.3348) H3B(0.3908) H1SA(0.141)
 H1SB(0.1161)
;
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.804