Synthesis and optical power limiting properties of heteroleptic Mo3S7 clusters.
Recatalá, David; Llusar, Rosa; Barlow, Adam; Wang, Genmiao; Samoc, Marek; Humphrey, Mark G.; Guschin, Artem L.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13163–13172; doi:10.1039/c5dt01244a

data_7035335
_publ_section_title
;
 Synthesis and optical power limiting properties of heteroleptic Mo3S7
 clusters.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13163
_journal_page_last               13172
_journal_paper_doi               10.1039/c5dt01244a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C12 H12 Br4 Mo3 N2 S7, Br, 0.83(C16 H36 N), 0.17(C16 H31 N), 0.17(C H2 Cl2), 0.17(C7 H8), 0.17(C Cl2), 0.17(C H2 Cl1.6)'
_chemical_formula_sum            'C29.67 H49.17 Br5 Cl0.93 Mo3 N3 S7'
_chemical_formula_weight         1392.76
_chemical_name_systematic        (Bu4N)[Mo3S7Br4(dmbpy).Br]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-11 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                71.8853(15)
_cell_angle_beta                 76.3237(14)
_cell_angle_gamma                70.0386(15)
_cell_formula_units_Z            12
_cell_length_a                   19.3605(3)
_cell_length_b                   25.9644(4)
_cell_length_c                   34.7600(5)
_cell_measurement_reflns_used    69651
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      27.1380
_cell_measurement_theta_min      3.1060
_cell_volume                     15442.6(4)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   -6.00   98.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436   57.0000   30.0000 104

  2 omega  -12.00   68.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436   57.0000  -90.0000 80

  3 omega  -71.00   50.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436  -57.0000  120.0000 121

  4 omega  -14.00   98.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436   38.0000 -180.0000 112

  5 omega  -53.00   53.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436  -77.0000  -90.0000 106

  6 omega  -20.00   61.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436  -99.0000   30.0000 81

  7 omega  -53.00   14.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3498   85.0000  -47.0000 67

  8 omega  -26.00  105.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436   77.0000 -180.0000 131

  9 omega  -20.00   61.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436  -99.0000 -120.0000 81

 10 omega  -24.00   94.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436   38.0000  -30.0000 118

 11 omega  -20.00   61.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4436  -99.0000   90.0000 81
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0332842000
_diffrn_orient_matrix_UB_12      -0.0079903000
_diffrn_orient_matrix_UB_13      0.0069229000
_diffrn_orient_matrix_UB_21      0.0177029000
_diffrn_orient_matrix_UB_22      -0.0252412000
_diffrn_orient_matrix_UB_23      -0.0066221000
_diffrn_orient_matrix_UB_31      0.0114492000
_diffrn_orient_matrix_UB_32      -0.0141802000
_diffrn_orient_matrix_UB_33      0.0194728000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            331374
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.784
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45126
_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            reddish
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       needle
_exptl_crystal_F_000             8124
_exptl_crystal_recrystallization_method
'Slow diffusion toluene/dichloromethane'
_exptl_crystal_size_max          0.4007
_exptl_crystal_size_mid          0.2194
_exptl_crystal_size_min          0.0933
_refine_diff_density_max         3.075
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2663
_refine_ls_number_reflns         60352
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0754P)^2^+200.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38699
_reflns_number_total             60352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01244a1.cif
_cod_data_source_block           str1571
_cod_depositor_comments
'Adding full bibliography for 7035335--7035338.cif.'
_cod_original_cell_volume        15442.7(5)
_cod_database_code               7035335
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C46 H80 N6 Br5 S7 Mo3'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-Cl31
 1.8 with sigma of 0.02
 Cl32-C30
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl43) = Uanis(Cl43)
4. Others
 Fixed Sof: Cl43(0.60178) Cl42(0.39822) C412(0.45) C417(0.55) Cl31(0.6)
5.a Secondary CH2 refined with riding coordinates:
 C413(H41A,H41B), C110(H11A,H11B), C105(H10A,H10B), C406(H40A,H40B), C202(H20A,
 H20B), C407(H40C,H40D), C109(H10C,H10D), C201(H20C,H20D), C102(H10E,H10F),
 C405(H40E,H40F), C101(H10G,H10H), C203(H20E,H20F), C114(H11F,H11G), C414(H41C,
 H41D), C410(H41E,H41F), C403(H40G,H40H), C107(H10I,H10J), C303(H30A,H30B),
 C111(H11H,H11I), C309(H30C,H30D), C313(H31A,H31B), C401(H40I,H40J), C501(H50A,
 H50B), C605(H60A,H60B), C509(H50C,H50D), C513(H51A,H51B), C210(H21A,H21B),
 C505(H50E,H50F), C113(H11J,H11K), C610(H61A,H61B), C613(H61C,H61D), C205(H20G,
 H20H), C409(H40N,H40O), C115(H11L,H11M), C510(H51C,H51D), C415(H41G,H41H),
 C514(H51E,H51F), C106(H10K,H10L), C207(H20I,H20J), C305(H30E,H30F), C301(H30G,
 H30H), C402(H40P,H40Q), C502(H50G,H50H), C503(H50I,H50J), C310(H31C,H31D),
 C302(H30I,H30J), C506(H50K,H50L), C206(H20K,H20L), C306(H30K,H30L), C609(H60C,
 H60D), C602(H60E,H60F), C511(H51G,H51H), C515(H51I,H51J), C211(H21C,H21D),
 C103(H10M,H10N), C601(H60G,H60H), C606(H60I,H60J), C607(H60K,H60L), C209(H20P,
 H20Q), C311(H31E,H31F), C611(H61E,H61F), C314(H31G,H31H), C307(H30P,H30Q),
 C507(H50M,H50N), C603(H60M,H60N), C614(H61G,H61H), C213(H21E,H21F), C315(H31L,
 H31M), C214(H21J,H21K), C215(H21L,H21M), C50(H50U,H50V), C615(H61L,H61M),
 C30(H30U,H30V)
5.b Aromatic/amide H refined with riding coordinates:
 C12C(H12C), C8E(H8E), C8C(H8C), C58(H58), C5E(H5E), C11D(H11Q), C2A(H2A),
 C12D(H12D), C68(H68), C5F(H5F), C8A(H8A), C74(H74), C1D(H1D), C8D(H8D),
 C1E(H1E), C8F(H8F), C5A(H5A), C12E(H12E), C1A(H1A), C5D(H5D), C1C(H1C),
 C12F(H12F), C1F(H1F), C2F(H2F), C11C(H11S), C12A(H12A), C1(H1), C2C(H2C),
 C2D(H2D), C6(H6), C11A(H11R), C11F(H11U), C5C(H5C), C11E(H11T), C2E(H2E),
 C174(H174), C22(H22), C26(H26), C23(H23), C25(H25), C24(H24)
5.c Idealised Me refined as rotating group:
 C112(H11C,H11D,H11E), C4C(H4CA,H4CB,H4CC), C4A(H4AA,H4AB,H4AC), C4D(H4DA,H4DB,
 H4DC), C10C(H10Z,H,HA), C408(H40K,H40L,H40M), C61(H61Q,H61R,H61S), C116(H11N,
 H11O,H11P), C4E(H4EA,H4EB,H4EC), C10D(H10U,H10V,H10W), C404(H40R,H40S,H40T),
 C204(H20M,H20N,H20O), C149(H14A,H14B,H14C), C4F(H4FA,H4FB,H4FC), C10E(H10,HB,
 HC), C10F(H0AA,HD,HE), C304(H30M,H30N,H30O), C516(H51K,H51L,H51M), C10A(H10X,
 H10Y,HF), C108(H10O,H10P,H10Q), C312(H31I,H31J,H31K), C416(H41I,H41J,H41K),
 C208(H20R,H20S,H20T), C608(H60O,H60P,H60Q), C604(H60R,H60S,H60T), C612(H61I,
 H61J,H61K), C512(H51N,H51O,H51P), C504(H50O,H50P,H50Q), C508(H50R,H50S,H50T),
 C308(H30R,H30S,H30T), C212(H21G,H21H,H21I), C316(H31N,H31O,H31P), C104(H10R,
 H10S,H10T), C216(H21N,H21O,H21P), C20(H20U,H20V,H20W), C616(H61N,H61O,H61P)
;
_shelx_res_checksum              10207
_olex2_submission_special_instructions 'No special instructions were received'