A Heteroaromatically Functionalized Hexamolybdate
Healey, Merinda; Best, Stephen; Goerigk, Lars; Ritchie, Chris; Inorganics 3 (2015) 82–; doi:10.3390/inorganics3020082

data_1520327
_publ_section_title
;
 A Heteroaromatically Functionalized Hexamolybdate
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              82
_journal_paper_doi               10.3390/inorganics3020082
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C16 H36 N, C13 H12 Br Mo6 N O18 S'
_chemical_formula_sum            'C45 H84 Br Mo6 N3 O18 S'
_chemical_formula_weight         1642.76
_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     direct
_audit_creation_date             2015-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8238(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.03023(16)
_cell_length_b                   16.9232(2)
_cell_length_c                   32.4507(5)
_cell_measurement_reflns_used    25171
_cell_measurement_temperature    130.01(10)
_cell_measurement_theta_max      76.9020
_cell_measurement_theta_min      4.8000
_cell_volume                     5985.78(15)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -16.00   33.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -      -40.8092   37.0000   60.0000 49

  2 omega   33.00   99.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       40.8092   37.0000  120.0000 66

  3 omega   54.00   80.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   -6.0000   55.4954 26

  4 omega   77.00  129.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000   60.0000 52

  5 omega  148.00  174.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   -6.0000   55.4954 26

  6 omega  145.00  172.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000    0.0000 27

  7 omega  147.00  173.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -90.0000 26

  8 omega  131.00  178.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -90.0000 47

  9 omega  146.00  178.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000 -180.0000 32

 10 omega  118.00  148.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -180.0000 30

 11 omega  119.00  145.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -150.0000 26

 12 omega  111.00  150.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000  -90.0000 39

 13 omega  109.00  137.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  111.0000 -180.0000 28

 14 omega   84.00  146.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 62

 15 omega  120.00  149.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  -90.0000 29

 16 omega  110.00  149.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -150.0000 39

 17 omega  109.00  138.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 29

 18 omega  100.00  136.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -76.0000  -72.5198 36

 19 omega   95.00  121.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000 -150.0000 26

 20 omega   91.00  116.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -150.0000 25

 21 omega   89.00  115.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 26

 22 omega   85.00  115.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 30

 23 omega   74.00  115.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -90.0000 41

 24 omega   81.00  107.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -82.0000  -95.9691 26

 25 omega   82.00  108.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000  -60.0000 26

 26 omega   91.00  117.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000    0.0000 26

 27 omega   90.00  116.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   30.0000 26

 28 omega  106.00  132.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -86.0000   62.4933 26

 29 omega  103.00  128.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000   60.0000 25

 30 omega   90.00  116.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  120.0000 26

 31 omega   85.00  115.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 30

 32 omega   74.00  100.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -63.0000   94.3951 26

 33 omega   65.00   92.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -39.0000   41.9902 27

 34 omega   89.00  119.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 30

 35 omega  108.00  147.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   -6.0000   55.4954 39

 36 omega   99.00  177.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   60.0000 78

 37 omega  142.00  174.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  120.0000 32

 38 omega  105.00  131.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000   30.0000 26

 39 omega  115.00  146.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 31

 40 omega   91.00  118.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -60.0000 27

 41 omega   58.00   94.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000 -180.0000 36

 42 omega   89.00  114.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -90.0000 25

 43 omega   84.00  173.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -60.0000 89

 44 omega   83.00  127.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   60.0000 44

 45 omega   61.00  114.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000    0.0000 53

 46 omega   64.00   94.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -86.0000   62.4933 30

 47 omega   69.00  110.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000    0.0000 41

 48 omega   91.00  116.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -30.0000 25

 49 omega   62.00  102.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  -30.0000 40

 50 omega   51.00   95.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -51.0000  -28.4478 44

 51 omega   51.00   87.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   30.0000 36

 52 omega   57.00  104.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   90.0000 47

 53 omega   63.00  112.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  150.0000 49

 54 omega   50.00   76.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  150.0000 26

 55 omega   44.00   69.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -63.0000   94.3951 25

 56 omega   35.00   79.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   30.0000 44

 57 omega   48.00   74.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 26

 58 omega   39.00   86.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 47

 59 omega   60.00   85.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 25

 60 omega   53.00  102.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  -90.0000 49

 61 omega   45.00   84.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000 -150.0000 39

 62 omega   38.00   63.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -76.0000  -72.5198 25

 63 omega   45.00  103.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  -90.0000 58

 64 omega   50.00   96.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -180.0000 46

 65 omega   44.00   78.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -150.0000 34

 66 omega   47.00   73.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 26

 67 omega   42.00   68.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -90.0000 26

 68 omega   37.00   97.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -150.0000 60

 69 omega   44.00   69.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 25

 70 omega   35.00   97.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -120.0000 62

 71 omega   39.00   98.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -90.0000 59

 72 omega   39.00   90.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -30.0000 51

 73 omega   46.00   76.00   1.0000    8.2900
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 30

 74 omega   29.00   82.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       40.8092 -125.0000  -90.0000 53

 75 omega   44.00   75.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -       40.8092 -125.0000 -180.0000 31

 76 omega  -49.00   33.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -      -40.8092   37.0000 -150.0000 82

 77 omega  -57.00  -26.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -      -40.8092  -37.0000   60.0000 31

 78 omega -115.00 -103.00   1.0000    2.0700
omega____ theta____ kappa____ phi______ frames
    -      -40.8092  -57.0000  -90.0000 12
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312702000
_diffrn_orient_matrix_UB_12      -0.0716694000
_diffrn_orient_matrix_UB_13      -0.0256696000
_diffrn_orient_matrix_UB_21      0.1290431000
_diffrn_orient_matrix_UB_22      -0.0037428000
_diffrn_orient_matrix_UB_23      0.0260331000
_diffrn_orient_matrix_UB_31      -0.0485277000
_diffrn_orient_matrix_UB_32      -0.0559874000
_diffrn_orient_matrix_UB_33      0.0311656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_laue_measured_fraction_full 0.991
_diffrn_reflns_laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            105913
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.284
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.658
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   analytical
_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)
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_colour            red
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.2905
_exptl_crystal_size_mid          0.1781
_exptl_crystal_size_min          0.0576
_refine_diff_density_max         3.864
_refine_diff_density_min         -3.320
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         12538
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1435P)^2^+14.6971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10120
_reflns_number_total             12538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s1.cif
_cod_data_source_block           mh1_178_2
_cod_original_cell_volume        5985.79(15)
_cod_database_code               1520327
_chemical_oxdiff_formula         Mo6O18N3C45H84S1Br
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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. Shared sites
{C15, Br1}
{C14, Br2}
3. Restrained distances
 C32-C34
 1.5 with sigma of 0.02
 C33-C35
 1.5 with sigma of 0.02
 C32-C30
 1.5 with sigma of 0.02
 C30-C33
 1.5 with sigma of 0.02
 C13-C15
 1.5 with sigma of 0.02
 C12-C14
 1.5 with sigma of 0.02
 C9-C11
 1.35 with sigma of 0.02
 C12-C13
 1.35 with sigma of 0.02
 C10-C12
 1.41 with sigma of 0.02
 C11-C13
 1.41 with sigma of 0.02
 C9-S1
 1.7 with sigma of 0.02
 S1-C12
 1.7 with sigma of 0.02
 C9-S2
 1.7 with sigma of 0.02
 S2-C13
 1.7 with sigma of 0.02
 C29-C31
 1.5 with sigma of 0.02
 C30-C29
 1.5 with sigma of 0.02
 C26-C25
 1.5 with sigma of 0.02
 C26-C25
 1.53 with sigma of 0.02
 C30-C34
 2.5 with sigma of 0.04
 C35-C30
 2.5 with sigma of 0.04
 C10-S2
 2.55 with sigma of 0.04
 S1-C13
 2.55 with sigma of 0.04
 S1-C11
 2.55 with sigma of 0.04
 C12-S2
 2.55 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uiso(C15) = Uiso(Br1)
Uiso(C14) = Uiso(Br2)
Uiso(S2) = Uiso(S1)
Uiso(C33) = Uiso(C35) = Uiso(C32) = Uiso(C34)
Uiso(C11) = Uiso(C10)
5. Others
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(C11)=Sof(H11)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(S1)=Sof(Br1)=1-
 FVAR(2)
 Sof(C10)=Sof(H10)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(S2)=Sof(Br2)=
 FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11)
6.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              92707
_shelx_hkl_checksum              71243
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-01-19
_olex2_submission_special_instructions 'No special instructions were received'