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_7035336
_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
'C10 H8 Br4 Mo3 N2 S7, Br, 0.5(C16 H35 N), 0.5(C H2 Cl2), 0.5(C16 N), 0.5(C7 H8)'
_chemical_formula_sum            'C30 H30.5 Br5 Cl Mo3 N3 S7'
_chemical_formula_weight         1380.31
_chemical_name_systematic        (Bu4N)[Mo3S7Br4(bpy).Br]
_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
_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                90
_cell_angle_beta                 108.499(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.19024(19)
_cell_length_b                   32.5907(6)
_cell_length_c                   14.5892(3)
_cell_measurement_reflns_used    24330
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      29.0120
_cell_measurement_theta_min      3.0230
_cell_volume                     5045.73(17)
_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      199.95(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    5.00   31.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000   60.0000 26

  2 omega  -89.00  -63.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000   30.0000 26

  3 omega   73.00   99.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191 -178.0000   30.0000 26

  4 omega  -48.00   30.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -57.0000 -150.0000 78

  5 omega  -66.00   37.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -77.0000  -30.0000 103

  6 omega  -64.00    4.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -37.0000    0.0000 68

  7 omega  -14.00   88.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191   37.0000    0.0000 102
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0194495000
_diffrn_orient_matrix_UB_12      0.0050634000
_diffrn_orient_matrix_UB_13      -0.0498406000
_diffrn_orient_matrix_UB_21      0.0131179000
_diffrn_orient_matrix_UB_22      -0.0203458000
_diffrn_orient_matrix_UB_23      -0.0111947000
_diffrn_orient_matrix_UB_31      -0.0625963000
_diffrn_orient_matrix_UB_32      -0.0058389000
_diffrn_orient_matrix_UB_33      -0.0042213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48304
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.835
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70550
_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    1.817
_exptl_crystal_description       needle
_exptl_crystal_F_000             2646
_exptl_crystal_recrystallization_method
'Slow diffusion toluene/dichloromethane'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.063
_refine_diff_density_max         3.293
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details
;
 Flack x determined using 7533 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         17681
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0807P)^2^+9.9051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                16496
_reflns_number_total             17681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01244a1.cif
_cod_data_source_block           str1473
_cod_depositor_comments
'Adding full bibliography for 7035335--7035338.cif.'
_cod_original_cell_volume        5045.73(16)
_cod_original_formula_sum        'C30 H30.50 Br5 Cl Mo3 N3 S7'
_cod_database_code               7035336
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C26 H44 N3 Br5 S7 Mo3'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C216-C215
 1.5 with sigma of 0.02
 C215-C216
 1.5 with sigma of 0.02
 C209-C210
 1.5 with sigma of 0.02
 C210-C211
 1.5 with sigma of 0.02
 C211-C212
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C216) = Uanis(C217)
4. Others
 Fixed Sof: C216(0.43) C217(0.57)
5.a Secondary CH2 refined with riding coordinates:
 C109(H10A,H10B), C101(H10C,H10D), C105(H10E,H10F), C113(H11A,H11B), C106(H10G,
 H10H), C102(H10I,H10J), C110(H11C,H11D), C114(H11E,H11F), C107(H10K,H10L),
 C103(H10M,H10N), C111(H11G,H11H), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C4'(H4'), C4(H4), C1(H1), C7(H7), C3'(H3'), C1'(H1'),
 C2'(H2'), C7'(H7'), C10'(H10'), C2(H2), C9(H9), C9'(H9'), C8(H8), C8'(H8'),
 C115(H115), C36(H36), C35(H35), C32(H32), C34(H34), C33(H33)
5.c Idealised Me refined as rotating group:
 C108(H10O,H10P,H10Q), C112(H11I,H11J,H11K), C104(H10R,H10S,H10T), C116(H11L,
 H11M,H11N), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              62321
_olex2_submission_special_instructions 'No special instructions were received'