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_7023246
_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_formula_moiety         'C28 H16 Mo2 N4 O2 S10, 2(C8 H20 N)'
_chemical_formula_sum            'C44 H56 Mo2 N6 O2 S10'
_chemical_formula_weight         1213.43
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2011.12.05 svn.r2101, GUI svn.r3974)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 114.965(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.411(2)
_cell_length_b                   9.4996(4)
_cell_length_c                   21.3573(15)
_cell_measurement_reflns_used    6896
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      29.3451
_cell_measurement_theta_min      2.8668
_cell_volume                     5409.5(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      220.0
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
1 omega -99.00 61.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- -11.5596 0.0000 60.0000 160

2 omega 66.00 91.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- 12.2627 77.0000 30.0000 25

3 omega 14.00 41.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- 12.2627 77.0000 30.0000 27

4 omega -14.00 24.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- 12.2627 37.0000 150.0000 38

5 omega -88.00 15.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- -11.5596 -37.0000 -120.0000 103

6 omega -38.00 19.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- -11.5596 37.0000 -120.0000 57

7 omega -74.00 -29.00 1.0000 22.0000
omega____ theta____ kappa____ phi______ frames
- -11.5596 133.0000 95.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0185296000
_diffrn_orient_matrix_UB_12      -0.0520297000
_diffrn_orient_matrix_UB_13      0.0162801000
_diffrn_orient_matrix_UB_21      0.0080034000
_diffrn_orient_matrix_UB_22      0.0054951000
_diffrn_orient_matrix_UB_23      -0.0269340000
_diffrn_orient_matrix_UB_31      0.0173347000
_diffrn_orient_matrix_UB_32      0.0532438000
_diffrn_orient_matrix_UB_33      0.0187443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31083
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.4411
_exptl_crystal_size_mid          0.0638
_exptl_crystal_size_min          0.0272
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+14.5716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                4140
_reflns_number_total             6874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51102b.txt
_cod_data_source_block           str1234
_cod_original_cell_volume        5409.7(6)
_cod_database_code               7023246
_chemical_oxdiff_formula         'C44 H56 O2 S10 N6 Mo2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H14 of C14, H9 of C9, {H10M,H10N} of C107, H7 of C7, {H10K,H10L} of C103,
H12 of C12, H8 of C8, {H10I,H10J} of C101, H11 of C11, H6 of C6, H13 of C13,
{H10G,H10H} of C105
At 1.5 times of:
{H10A,H10B,H10C} of C104, {H10D,H10E,H10F} of C106, {H10R,H10S,H10T} of
C102, {H10O,H10P,H10Q} of C108
2.a Secondary CH2 refined with riding coordinates:
C105(H10G,H10H), C101(H10I,H10J), C103(H10K,H10L), C107(H10M,H10N)
2.b Aromatic/amide H refined with riding coordinates:
C14(H14), C9(H9), C13(H13), C6(H6), C11(H11), C8(H8), C12(H12), C7(H7)
2.c Idealised Me refined as rotating group:
C104(H10A,H10B,H10C), C106(H10D,H10E,H10F), C108(H10O,H10P,H10Q), C102(H10R,
H10S,H10T)
;