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_7029520
_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 O4 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C18 H20 Cl4 Mo2 N4 O4 S4'
_chemical_formula_weight         818.30
_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                 110.31(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.101(4)
_cell_length_b                   20.553(10)
_cell_length_c                   7.445(4)
_cell_measurement_reflns_used    3794
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.39
_cell_volume                     1306.0(11)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_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 0.996
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7377
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0380P)^2^+3.0059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2416
_reflns_number_total             2981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00297k2.cif
_cod_data_source_block           4a_CH2Cl2_100K
_cod_original_cell_volume        1305.9(11)
_cod_database_code               7029520
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.022) H2B(0.022) H3A(0.019) H3B(0.019) H6A(0.028) H6B(0.028)
 H7A(0.026) H7B(0.026) H9AA(0.055) H9AB(0.055) H9BC(0.055) H9BD(0.055)
 H9CE(0.055) H9CF(0.055)
 Fixed X: H2A(0.745) H2B(0.5645) H3A(0.5305) H3B(0.7176) H6A(1.0288)
 H6B(1.0753) H7A(1.0391) H7B(0.9921) H9AA(0.7947) H9AB(0.8307) H9BC(0.7774)
 H9BD(0.8099) H9CE(0.8267) H9CF(0.7974)
 Fixed Y: H2A(0.2969) H2B(0.2736) H3A(0.3168) H3B(0.3267) H6A(0.6062)
 H6B(0.5358) H7A(0.5735) H7B(0.6438) H9AA(0.6561) H9AB(0.6829) H9BC(0.7147)
 H9BD(0.6465) H9CE(0.6938) H9CF(0.6515)
 Fixed Z: H2A(0.3424) H2B(0.2717) H3A(0.5322) H3B(0.62) H6A(0.2326)
 H6B(0.3319) H7A(0.598) H7B(0.4986) H9AA(0.8087) H9AB(1.0212) H9BC(0.7749)
 H9BD(0.8859) H9CE(1.022) H9CF(0.8313)
;
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.681
_shelxl_version_number           2013-3