Dithiolene dimetallic molybdenum(V) complexes displaying intraligand charge transfer (ILCT) emission.
Recatalá, David; Gushchin, Artem L.; Llusar, Rosa; Galindo, F.; Brylev, Konstantin A.; Ryzhikov, Maxim R.; Kitamura, Noboru; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12947–12955; doi:10.1039/c3dt51102b

data_7023247
_publ_section_title
;
 Dithiolene dimetallic molybdenum(V) complexes displaying intraligand
 charge transfer (ILCT) emission.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12947
_journal_page_last               12955
_journal_paper_doi               10.1039/c3dt51102b
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H14 N2 S4 Sn, C4 O'
_chemical_formula_sum            'C20 H15 N2 O S4 Sn'
_chemical_formula_weight         546.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.706(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.90185(15)
_cell_length_b                   15.7670(4)
_cell_length_c                   10.3916(3)
_cell_measurement_reflns_used    7089
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      28.8509
_cell_measurement_theta_min      2.9514
_cell_volume                     1128.46(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
1 omega -55.00 48.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- 16.5978 -57.0000 0.0000 206

2 omega -73.00 44.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- 16.5978 -77.0000 120.0000 234

3 omega 35.00 80.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- -15.9728 178.0000 0.0000 90

4 omega 35.00 113.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- 16.5978 178.0000 -30.0000 156

5 omega -21.00 28.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- 16.5978 38.0000 0.0000 98

6 omega -20.00 101.00 0.5000 2.0000
omega____ theta____ kappa____ phi______ frames
- 16.5978 57.0000 120.0000 242
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0103943000
_diffrn_orient_matrix_UB_12      -0.0010617000
_diffrn_orient_matrix_UB_13      -0.0683590000
_diffrn_orient_matrix_UB_21      -0.1001395000
_diffrn_orient_matrix_UB_22      0.0095206000
_diffrn_orient_matrix_UB_23      0.0021412000
_diffrn_orient_matrix_UB_31      0.0214508000
_diffrn_orient_matrix_UB_32      0.0439525000
_diffrn_orient_matrix_UB_33      -0.0020168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12798
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.058(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                4811
_reflns_number_total             5281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51102b.txt
_cod_data_source_block           exp_458
_cod_database_code               7023247
_chemical_oxdiff_formula         'C16 H14 N2 S4 Sn'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H13 of C13, H16 of C16, H11 of C11, H15 of C15, H14 of C14, H8 of C8, H10
of C10, H9 of C9
At 1.5 times of:
{H2A,H2B,H2C} of C2, {H1A,H1B,H1C} of C1
2. Others
Fixed Sof: O1(0.614) O2(0.386)
3.a Aromatic/amide H refined with riding coordinates:
C13(H13), C16(H16), C11(H11), C15(H15), C14(H14), C8(H8), C10(H10), C9(H9)
3.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;