Boronic acid and boronic ester containing polyoxometalates.
Karoui, Hedi; Ritchie, Chris; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18838–18841; doi:10.1039/c6dt04197c

data_7041170
_publ_section_title
;
 Boronic acid and boronic ester containing polyoxometalates.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18838
_journal_page_last               18841
_journal_paper_doi               10.1039/c6dt04197c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'B2 C22 Mn Mo6 N2 O28'
_chemical_formula_sum            'C70 H134 B2 Mn Mo6 N5 O28'
_chemical_formula_weight         2146.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-27
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2016-07-28 deposited with the CCDC.
2016-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.407(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0713(6)
_cell_length_b                   14.3578(5)
_cell_length_c                   28.5472(15)
_cell_measurement_reflns_used    10359
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      75.7230
_cell_measurement_theta_min      3.5680
_cell_volume                     9837.1(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      air
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   37.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 47

  2 omega  116.00  142.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000   90.0000 26

  3 omega  111.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000   90.0000 39

  4 omega  119.00  147.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  120.0000 28

  5 omega  124.00  149.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  150.0000 25

  6 omega  107.00  136.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000   60.0000 29

  7 omega   64.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  150.0000 26

  8 omega   58.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000   90.0000 44

  9 omega   58.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000   30.0000 36

 10 omega  100.00  144.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000  -90.0000 44

 11 omega  101.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  111.0000 -120.0000 76

 12 omega  117.00  143.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000 -180.0000 26

 13 omega   95.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  125.0000 -150.0000 30

 14 omega  113.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -120.0000 37

 15 omega  110.00  135.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -180.0000 25

 16 omega   57.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -120.0000 41

 17 omega   58.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000  -90.0000 47

 18 omega   60.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  178.0000 -180.0000 34

 19 omega  113.00  173.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   37.0000   30.0000 60

 20 omega  153.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000  -60.0000 25

 21 omega  124.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000 -120.0000 53

 22 omega  120.00  146.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   37.0000 -150.0000 26

 23 omega   98.00  149.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -12.0000  -60.0000 51

 24 omega  115.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -12.0000    0.0000 43

 25 omega  130.00  156.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000   30.0000 26

 26 omega  126.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   50.0000   90.0000 49

 27 omega  102.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000    0.0000 74

 28 omega  110.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000   30.0000 38

 29 omega  124.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000   60.0000 26

 30 omega  106.00  132.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000   90.0000 26

 31 omega   91.00  127.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000  150.0000 36

 32 omega   74.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000   60.0000 40

 33 omega   79.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000   30.0000 29

 34 omega   69.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -60.0000 44

 35 omega  117.00  143.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -91.0000  -90.0000 26

 36 omega  128.00  155.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000  -60.0000 27

 37 omega  121.00  161.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -91.0000 -150.0000 40

 38 omega   76.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000  -60.0000 26

 39 omega   64.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000   25.0000 -120.0000 38

 40 omega   59.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -37.0000 -180.0000 32

 41 omega   71.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -54.0000 -150.9981 26

 42 omega   67.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -37.0000 -150.0000 25

 43 omega   63.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -50.0000 -150.0000 30

 44 omega   73.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000  -90.0000 26

 45 omega   73.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -150.0000 43

 46 omega   73.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -180.0000 43

 47 omega   56.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  -57.0000 -180.0000 26

 48 omega   29.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000 -125.0000 -180.0000 92

 49 omega   57.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -120.0000 57

 50 omega   66.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000    0.0000 50

 51 omega   66.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000   90.0000 50

 52 omega   73.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000  150.0000 25

 53 omega   65.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -25.0000  120.0000 25

 54 omega   57.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -50.0000   60.0000 36

 55 omega   47.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000   30.0000 26

 56 omega   39.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -37.0000   90.0000 25

 57 omega   36.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -25.0000  120.0000 26

 58 omega   36.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -50.0000  120.0000 59

 59 omega   43.00   73.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -25.0000    0.0000 30

 60 omega   58.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -25.0000  -60.0000 26

 61 omega   37.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -37.0000    0.0000 47

 62 omega   37.00   63.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -12.0000  -60.0000 26

 63 omega   42.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -37.0000  -90.0000 39

 64 omega   50.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -91.0000 -150.0000 52

 65 omega   37.00   62.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000 -150.0000 25

 66 omega   38.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -90.0000 43

 67 omega   34.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -60.0000 25

 68 omega   37.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  -30.0000 68

 69 omega   33.00   58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -77.0000   60.0000 25

 70 omega   33.00   58.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -63.0000   90.0000 25

 71 omega   43.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000 -111.0000  120.0000 54

 72 omega   35.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -48.0000  -31.9768 59

 73 omega   32.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      118.0000  -91.0000 -120.0000 81

 74 omega    1.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 25

 75 omega  -25.00   46.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       59.0000  -57.0000 -180.0000 71

 76 omega  -34.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000    0.0000 53

 77 omega  -27.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   37.0000   60.0000 39

 78 omega  -49.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000   37.0000  -60.0000 64

 79 omega  -45.00  -20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  139.0000   24.0000 25

 80 omega    1.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 25

 81 omega  -60.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 25

 82 omega  -94.00  -66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 28

 83 omega -101.00  -73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000 -125.0000  -60.0000 28

 84 omega -140.00  -29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -59.0000  -57.0000  -30.0000 111
;
_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      -0.0076278000
_diffrn_orient_matrix_UB_12      -0.0102638000
_diffrn_orient_matrix_UB_13      -0.0538486000
_diffrn_orient_matrix_UB_21      -0.0419742000
_diffrn_orient_matrix_UB_22      -0.0794828000
_diffrn_orient_matrix_UB_23      0.0053681000
_diffrn_orient_matrix_UB_31      -0.0479836000
_diffrn_orient_matrix_UB_32      0.0712572000
_diffrn_orient_matrix_UB_33      -0.0016859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            78795
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.742
_diffrn_reflns_theta_min         3.448
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.646
_exptl_absorpt_correction_T_max  0.494
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       plates
_exptl_crystal_F_000             4400
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.2308
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1313
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         10426
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.926
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1533P)^2^+6.6988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2487
_refine_ls_wR_factor_ref         0.2647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7161
_reflns_number_total             10426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04197c2.cif
_cod_data_source_block           hk-2-170-2-new
_cod_depositor_comments
'Adding full bibliography for 7041170--7041172.cif.'
_cod_database_code               7041170
_chemical_oxdiff_formula         'Mo6 Mn1 O21 C80'
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.275
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C11'-C8'
 1.4 with sigma of 0.02
 C8'-C9'
 1.4 with sigma of 0.02
 C9'-C10'
 1.4 with sigma of 0.02
 C10'-C6'
 1.4 with sigma of 0.02
 C6'-C7'
 1.4 with sigma of 0.02
 C8-C7
 1.39 with sigma of 0.02
 C10-C8
 1.39 with sigma of 0.02
 C6-C9
 1.39 with sigma of 0.02
 C9-C7
 1.39 with sigma of 0.02
 C10-C11
 1.39 with sigma of 0.02
 C6-C11
 1.39 with sigma of 0.02
 C11-B1
 1.55 with sigma of 0.02
 C7'-B1'
 1.55 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 C5'-C6
 1.5 with sigma of 0.02
 N1'-C5
 1.25 with sigma of 0.02
 N1-C5'
 1.25 with sigma of 0.02
 O12-C3
 1.5 with sigma of 0.02
 O12-C3'
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 C1'-C4
 1.5 with sigma of 0.02
 C2-C4
 1.5 with sigma of 0.02
 C1-C4'
 1.5 with sigma of 0.02
 C2'-C4'
 1.5 with sigma of 0.02
 C4'-C3'
 1.5 with sigma of 0.02
 C3-O12
 1.5 with sigma of 0.02
 C8'-C7'
 2.5 with sigma of 0.04
 C11'-C6'
 2.5 with sigma of 0.04
 C6'-C9'
 2.5 with sigma of 0.04
 C3-N1
 2.5 with sigma of 0.04
 N1'-C1
 2.5 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uiso(B1') = Uiso(B1)
Uiso(O14') = Uiso(O13') = Uiso(O13) = Uiso(O14)
Uiso(N1) = Uiso(N1') = Uiso(C5) = Uiso(C5')
Uiso(C6) = Uiso(C6') = Uiso(C11) = Uiso(C10') = Uiso(C10) = Uiso(C9') =
Uiso(C9) = Uiso(C8') = Uiso(C8) = Uiso(C7) = Uiso(C7') = Uiso(C11')
Uiso(B1') = Uiso(B1)
Uiso(O14') = Uiso(O13') = Uiso(O14) = Uiso(O13)
3. Others
 Fixed Sof: O13(0.5) O14(0.5) N1'(0.5) C4'(0.5) C1(0.5) C5(0.5) C6(0.5)
 C11(0.5) C10(0.5) C9(0.5) C8(0.5) C7(0.5) C3'(0.5) C2'(0.5) B1(0.5) O13'(0.5)
 O14'(0.5) N1(0.5) C2(0.5) C3(0.5) C4(0.5) C5'(0.5) C7'(0.5) C8'(0.5) C9'(0.5)
 C10'(0.5) C11'(0.5) C6'(0.5) C1'(0.5) B1'(0.5)
4.a Fitted hexagon refined as free rotating group:
 C6(C11,C10,C9,C8,C7), C7'(C8',C9',C10',C11',C6')
;
_shelx_res_checksum              28984
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-04-17
_olex2_submission_special_instructions 'No special instructions were received'