New sterically encumbered arylimido hexamolybdates for organic oxidation reactions
Jangir, Ritambhara; Antony, Rajendran; Murugavel, Ramaswamy; New J. Chem. 40 (2016) 1004–; doi:10.1039/C5NJ02330K

data_7055238
_publ_section_title
;
 New sterically encumbered arylimido hexamolybdates for organic oxidation
 reactions
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1004
_journal_paper_doi               10.1039/C5NJ02330K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C12 H16 Br Mo6 N O18, 2(C16 H36 N)'
_chemical_formula_sum            'C44 H88 Br Mo6 N3 O18'
_chemical_formula_weight         1602.72
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-22
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.01.23 svn.r2171, GUI svn.r4051)
;
_audit_update_record
;
2015-11-29 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                99.315(3)
_cell_angle_beta                 99.810(3)
_cell_angle_gamma                95.905(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8380(4)
_cell_length_b                   12.3065(4)
_cell_length_c                   20.7813(8)
_cell_measurement_reflns_used    14452
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.0290
_cell_measurement_theta_min      4.6103
_cell_volume                     2917.29(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 8.1207
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -50.00   26.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000   30.0000 76

  2 omega  -55.00   35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000 -120.0000 90

  3 omega -104.00  -17.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -50.0000   90.0000 87

  4 omega   11.00  107.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   19.0000 -120.0000 96

  5 omega  -17.00   41.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -46.0000   40.0000 58

  6 omega   34.00  123.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 89

  7 omega   73.00  100.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 27

  8 omega    4.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -69.0000  -55.0000 72

  9 omega   38.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  120.0000 27

 10 omega   45.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -46.0000   40.0000 31

 11 omega   46.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -122.0000 -139.0000 55

 12 omega   68.00  113.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 45

 13 omega   35.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 58

 14 omega   42.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -64.0000  150.0000 79

 15 omega   36.00   78.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 42

 16 omega   67.00   92.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 25

 17 omega   36.00   62.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 26

 18 omega   37.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 56

 19 omega   40.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -60.0000 27

 20 omega  130.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 44

 21 omega   80.00  119.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -122.0000 -122.0000 39

 22 omega   87.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 40

 23 omega   67.00  110.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 43

 24 omega   41.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 45

 25 omega  101.00  127.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 26

 26 omega   35.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 46

 27 omega   47.00   86.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 39

 28 omega   42.00   89.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -64.0000  -30.0000 47

 29 omega   77.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -64.0000 -150.0000 52

 30 omega   50.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 43

 31 omega   57.00   82.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 25

 32 omega  116.00  176.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 60

 33 omega   53.00   78.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -152.0000 -102.0000 25

 34 omega   48.00  104.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  -90.0000 56

 35 omega   41.00  112.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -64.0000   60.0000 71
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1056325000
_diffrn_orient_matrix_UB_12      -0.0899222000
_diffrn_orient_matrix_UB_13      -0.0114463000
_diffrn_orient_matrix_UB_21      -0.0182391000
_diffrn_orient_matrix_UB_22      -0.0004101000
_diffrn_orient_matrix_UB_23      -0.0752356000
_diffrn_orient_matrix_UB_31      0.0792100000
_diffrn_orient_matrix_UB_32      -0.0911617000
_diffrn_orient_matrix_UB_33      -0.0080578000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22568
_diffrn_reflns_theta_full        71.16
_diffrn_reflns_theta_max         71.16
_diffrn_reflns_theta_min         4.61
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    11.614
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.4111
_exptl_crystal_size_mid          0.1961
_exptl_crystal_size_min          0.0607
_refine_diff_density_max         1.582
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         11000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+4.1438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                10452
_reflns_number_total             11000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02330k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7055238--7055240.cif.'
_cod_database_code               7055238
_chemical_oxdiff_formula         'C44 H88 Br1 Mo6 N3 O18'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49