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_7035338
_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 Cl4 Mo3 N2 S7, Cl, C16 H35 N, 3(C H2 Cl2)'
_chemical_formula_sum            'C31 H53 Cl11 Mo3 N3 S7'
_chemical_formula_weight         1369.95
_chemical_name_systematic        (Bu4N)[Mo3S7Cl4(dmbpy).Cl]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-11
_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                 103.4323(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8174(2)
_cell_length_b                   19.3711(3)
_cell_length_c                   20.0877(3)
_cell_measurement_reflns_used    24878
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.2200
_cell_measurement_theta_min      3.1310
_cell_volume                     5229.56(14)
_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(2)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -91.00  -12.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -19.0000  120.0000 79

  2 omega  -20.00   24.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000 -120.0000 44

  3 omega  -93.00  -60.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000  -90.0000 33

  4 omega  -20.00   11.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000   30.0000 31

  5 omega  -11.00   15.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000  150.0000 26

  6 omega  -85.00  -52.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -57.0000   30.0000 33

  7 omega -100.00  -68.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000 -180.0000 32

  8 omega    7.00   34.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -57.0000   90.0000 27

  9 omega  -37.00    4.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   37.0000  -60.0000 41

 10 omega  -42.00   64.00   1.0000   28.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   66.0000  146.0000 106
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0516035000
_diffrn_orient_matrix_UB_12      -0.0051872000
_diffrn_orient_matrix_UB_13      0.0028258000
_diffrn_orient_matrix_UB_21      -0.0002727000
_diffrn_orient_matrix_UB_22      -0.0274902000
_diffrn_orient_matrix_UB_23      0.0232799000
_diffrn_orient_matrix_UB_31      -0.0110097000
_diffrn_orient_matrix_UB_32      -0.0236262000
_diffrn_orient_matrix_UB_33      -0.0277201000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_laue_measured_fraction_full 0.971
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50572
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61115
_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    1.740
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_recrystallization_method
'Slow diffusion toluene/dichloromethane'
_exptl_crystal_size_max          0.4689
_exptl_crystal_size_mid          0.1936
_exptl_crystal_size_min          0.0702
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0484P)^2^+21.6496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7771
_reflns_number_total             9195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01244a1.cif
_cod_data_source_block           str1464
_cod_depositor_comments
'Adding full bibliography for 7035335--7035338.cif.'
_cod_original_cell_volume        5229.55(14)
_cod_database_code               7035338
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C28 H48 N3 S7 Cl5 Mo3'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H11(0.043) H10A(0.075) H10B(0.075) H12(0.045) H10C(0.107)
 H10D(0.107) H8(0.038) H10U(0.055) H10V(0.055) H10W(0.055) H2(0.059) H4A(0.089)
 H4B(0.089) H4C(0.089) H10E(0.081) H10F(0.081) H1(0.053) H10G(0.095)
 H10H(0.095) H5(0.045) H10I(0.071) H10J(0.071) H10K(0.086) H10L(0.086)
 H10M(0.145) H10N(0.145) H10O(0.145) H11A(0.125) H11B(0.125) H10P(0.092)
 H10Q(0.092) H11C(0.129) H11D(0.129) H11E(0.095) H11F(0.095) H10R(0.157)
 H10S(0.157) H10T(0.157) H11G(0.181) H11H(0.181) H115(0.211) H11I(0.389)
 H11J(0.389) H11K(0.389) H30A(0.122) H30B(0.122) H11L(0.252) H11M(0.252)
 H11N(0.252) H20A(0.178) H20B(0.178) H40A(0.424) H40B(0.424)
 Fixed X: H11(0.171) H10A(0.7057) H10B(0.7955) H12(0.2081) H10C(0.8132)
 H10D(0.8994) H8(0.1085) H10U(0.0655) H10V(0.1018) H10W(0.1781) H2(0.1322)
 H4A(0.0889) H4B(0.1338) H4C(0.0211) H10E(0.9134) H10F(0.9221) H1(0.1784)
 H10G(0.963) H10H(0.9553) H5(0.1009) H10I(0.7955) H10J(0.7893) H10K(0.6328)
 H10L(0.7215) H10M(0.8409) H10N(0.9407) H10O(0.8486) H11A(0.8944) H11B(0.9856)
 H10P(0.5857) H10Q(0.6761) H11C(0.8106) H11D(0.7968) H11E(0.6823) H11F(0.6832)
 H10R(0.5178) H10S(0.5267) H10T(0.6051) H11G(1) H11H(0.9144) H115(0.6108)
 H11I(0.613) H11J(0.7287) H11K(0.6838) H30A(-0.1935) H30B(-0.2522) H11L(1.0957)
 H11M(1.01) H11N(1.0447) H20A(0.1343) H20B(0.159) H40A(0.994) H40B(1.005)
 Fixed Y: H11(0.9558) H10A(0.5038) H10B(0.4548) H12(0.8714) H10C(0.5062)
 H10D(0.5573) H8(0.8091) H10U(0.976) H10V(0.925) H10W(0.9741) H2(0.5125)
 H4A(0.5251) H4B(0.5914) H4C(0.5895) H10E(0.6092) H10F(0.5372) H1(0.5585)
 H10G(0.5913) H10H(0.6643) H5(0.7033) H10I(0.569) H10J(0.6418) H10K(0.4707)
 H10L(0.4194) H10M(0.6977) H10N(0.6743) H10O(0.6246) H11A(0.4235) H11B(0.4739)
 H10P(0.4095) H10Q(0.3593) H11C(0.6544) H11D(0.6898) H11E(0.5759) H11F(0.6078)
 H10R(0.3672) H10S(0.309) H10T(0.3137) H11G(0.381) H11H(0.417) H115(0.6896)
 H11I(0.7509) H11J(0.7431) H11K(0.7915) H30A(0.6264) H30B(0.6731) H11L(0.4624)
 H11M(0.5104) H11N(0.4475) H20A(1.0283) H20B(0.954) H40A(0.8731) H40B(0.7951)
 Fixed Z: H11(0.1826) H10A(0.3935) H10B(0.3932) H12(0.2633) H10C(0.2469)
 H10D(0.2781) H8(0.0385) H10U(0.0512) H10V(0.0014) H10W(0.0488) H2(0.0946) H4A(-
 0.0272) H4B(-0.0533) H4C(-0.0512) H10E(0.3846) H10F(0.4206) H1(0.2011)
 H10G(0.5311) H10H(0.4968) H5(0.0181) H10I(0.4754) H10J(0.4401) H10K(0.2793)
 H10L(0.2817) H10M(0.559) H10N(0.6085) H10O(0.5933) H11A(0.3313) H11B(0.347)
 H10P(0.3663) H10Q(0.3714) H11C(0.2571) H11D(0.3249) H11E(0.2667) H11F(0.3383)
 H10R(0.2543) H10S(0.3096) H10T(0.2645) H11G(0.2667) H11H(0.2129) H115(0.2489)
 H11I(0.1732) H11J(0.185) H11K(0.2326) H30A(0.0286) H30B(0.0695) H11L(0.2668)
 H11M(0.2276) H11N(0.19) H20A(0.4236) H20B(0.4002) H40A(0.4712) H40B(0.4966)
;
_shelx_res_checksum              13650
_olex2_submission_special_instructions 'No special instructions were received'