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_7035337
_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 H8 Br4 Mo3 N2 S7, Br, C14.75 H28.25 N'
_chemical_formula_sum            'C26.75 H36.25 Br5 Mo3 N3 S7'
_chemical_formula_weight         1311.63
_chemical_name_systematic        (Bu4N)[Mo3S7Br4(phen).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             2015-01-26
_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                71.325(3)
_cell_angle_beta                 79.119(2)
_cell_angle_gamma                65.163(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9690(3)
_cell_length_b                   12.7039(4)
_cell_length_c                   16.6526(5)
_cell_measurement_reflns_used    16930
_cell_measurement_temperature    200.05(10)
_cell_measurement_theta_max      72.0290
_cell_measurement_theta_min      3.9510
_cell_volume                     2172.55(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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      200.05(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega -104.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -99.0000   30.0000 25

  2 omega    0.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687   77.0000   30.0000 26

  3 omega  -44.00  -18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687   77.0000   30.0000 26

  4 omega  -39.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687   37.0000  -90.0000 81

  5 omega -125.00  -88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -99.0000 -120.0000 37

  6 omega -119.00   -1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -57.0000  120.0000 118

  7 omega   79.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3687 -178.0000 -150.0000 26

  8 omega   64.00  132.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3687  178.0000 -180.0000 68

  9 omega -104.00   18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000   77.0000  -30.0000 122

 10 omega   29.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -30.0000  -60.0000 59

 11 omega   79.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222 -111.0000 -120.0000 35

 12 omega   53.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -45.0000   30.0000 43

 13 omega   38.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -94.0000   60.0000 67

 14 omega   57.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  178.0000   60.0000 25

 15 omega   31.00   56.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222 -111.0000 -120.0000 25

 16 omega   27.00   74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -30.0000    0.0000 47

 17 omega   26.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -30.0000   90.0000 60

 18 omega   42.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222 -111.0000   30.0000 64

 19 omega   48.00  146.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -77.0000  120.0000 98

 20 omega  103.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  178.0000   60.0000 37

 21 omega   97.00  149.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  178.0000  -90.0000 52

 22 omega   64.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -30.0000 -150.0000 26

 23 omega   61.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -30.0000 -120.0000 29

 24 omega  113.00  147.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -77.0000  150.0000 34

 25 omega   26.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222  -15.0000  120.0000 147

 26 omega -128.00    3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -77.0000  -60.0000 131

 27 omega -125.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -99.0000    0.0000 46

 28 omega -121.00    1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -37.0000  150.0000 122

 29 omega -121.00    0.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687  -57.0000   30.0000 121

 30 omega -126.00  -52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.3687 -157.0000  -20.0000 74

 31 omega   57.00  133.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3687  178.0000   90.0000 76

 32 omega   57.00  133.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.3687  178.0000  -60.0000 76

 33 omega -155.00 -106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -61.0000 -180.0000 49

 34 omega -162.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -77.0000  -90.0000 131

 35 omega -162.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -77.0000   30.0000 131

 36 omega -162.00  -31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.5000  -77.0000  120.0000 131

 37 omega   70.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222   77.0000  -60.0000 108

 38 omega   74.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222   45.0000   90.0000 104

 39 omega   73.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222   61.0000  150.0000 105

 40 omega   65.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222   30.0000   30.0000 113

 41 omega   20.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6222   15.0000  -60.0000 158
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0123281000
_diffrn_orient_matrix_UB_12      -0.0196962000
_diffrn_orient_matrix_UB_13      0.0969515000
_diffrn_orient_matrix_UB_21      0.1224330000
_diffrn_orient_matrix_UB_22      0.0150460000
_diffrn_orient_matrix_UB_23      -0.0046034000
_diffrn_orient_matrix_UB_31      -0.0710962000
_diffrn_orient_matrix_UB_32      0.1365630000
_diffrn_orient_matrix_UB_33      -0.0123935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31156
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         72.237
_diffrn_reflns_theta_min         2.807
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_description       needle
_exptl_crystal_F_000             1262
_exptl_crystal_recrystallization_method
'Slow diffusion toluene/dichloromethane'
_exptl_crystal_size_max          0.5229
_exptl_crystal_size_mid          0.2075
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.752
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8395
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0538
_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^)+(0.1100P)^2^+5.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7218
_reflns_number_total             8395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01244a1.cif
_cod_data_source_block           str1474
_cod_depositor_comments
'Adding full bibliography for 7035335--7035338.cif.'
_cod_original_cell_volume        2172.55(12)
_cod_database_code               7035337
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H44 N3 Br5 S7 Mo3'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C103-C104
 1.5 with sigma of 0.02
 C108-C107
 1.5 with sigma of 0.02
 C111-C112
 1.5 with sigma of 0.02
3. Others
 Fixed Sof: C112(0.75) H11N(0.75) H11O(0.75) H11P(0.75) C108(0.5) H10I(0.5)
 H10J(0.5) H10K(0.5) C104(0.5) H10N(0.5) H10O(0.5) H10P(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C114(H11A,H11B), C105(H10A,H10B), C113(H11C,H11D), C106(H10C,H10D), C110(H11E,
 H11F), C111(H11G,H11H), C107(H10E,H10F), C115(H11I,H11J), C102(H10G,H10H),
 C103(H10L,H10M)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C8(H8), C3(H3), C6(H6), C2(H2), C5(H5), C9(H9)
4.c Idealised Me refined as rotating group:
 C116(H11K,H11L,H11M), C112(H11N,H11O,H11P), C108(H10I,H10J,H10K), C104(H10N,
 H10O,H10P)
;
_shelx_res_checksum              69770
_olex2_submission_special_instructions 'No special instructions were received'