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_7041171
_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 C25.57 Mn Mo6 N2 O27.46, C26 H34 B2 Mn Mo6 N2 O28, 3.79(C14.5 N), 1.33(C3 N O)'
_chemical_formula_sum            'C148 H284 B4 Mn2 Mo12 N10 O56'
_chemical_formula_weight         4404.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-28
_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                 93.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.8863(8)
_cell_length_b                   24.7348(7)
_cell_length_c                   18.1665(6)
_cell_measurement_reflns_used    2643
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      44.0420
_cell_measurement_theta_min      4.7870
_cell_volume                     10269.7(6)
_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 1.000
_diffrn_measurement_details
;
  1 omega    3.00   61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  -30.0000 58

  2 omega  -23.00    2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  -30.0000 25

  3 omega  100.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442  125.0000 -120.0000 26

  4 omega   97.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442  125.0000 -180.0000 34

  5 omega   51.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442   77.0000 -120.0000 107

  6 omega   29.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442  -94.0000  -30.0000 77

  7 omega   16.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442  -30.0000  -60.0000 67

  8 omega   16.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       81.8442  -61.0000  120.0000 85

  9 omega  -69.00  -34.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  150.0000 35

 10 omega  -86.00  -59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 27

 11 omega  -85.00  -35.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 50
;
_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      -0.0568320000
_diffrn_orient_matrix_UB_12      -0.0301000000
_diffrn_orient_matrix_UB_13      0.0161055000
_diffrn_orient_matrix_UB_21      -0.0121882000
_diffrn_orient_matrix_UB_22      -0.0096815000
_diffrn_orient_matrix_UB_23      -0.0832115000
_diffrn_orient_matrix_UB_31      0.0340975000
_diffrn_orient_matrix_UB_32      -0.0536423000
_diffrn_orient_matrix_UB_33      0.0059941000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1042
_diffrn_reflns_av_unetI/netI     0.1447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26623
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        50.436
_diffrn_reflns_theta_max         50.436
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.338
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.556
_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_density_diffrn    1.424
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.1476
_exptl_crystal_size_mid          0.0428
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.654
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.1071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2975
_refine_ls_wR_factor_ref         0.3789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5182
_reflns_number_total             10748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04197c2.cif
_cod_data_source_block           cr1_184_02
_cod_depositor_comments
'Adding full bibliography for 7041170--7041172.cif.'
_cod_original_cell_volume        10269.6(6)
_cod_database_code               7041171
_chemical_oxdiff_formula         'Mo6 Mn1 O24 C80 N2'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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
 Mo06-O31
 1.75 with sigma of 0.02
 C16-C019
 1.5 with sigma of 0.02
 C019-C16
 1.5 with sigma of 0.02
 O38-C16
 1.4 with sigma of 0.02
 N4AA-C7AA
 1.4 with sigma of 0.02
 C7-N4AA
 1.4 with sigma of 0.02
 C1-N4AA
 1.3 with sigma of 0.02
 O1-C1
 1.25 with sigma of 0.02
 N5BA-C9
 1.5 with sigma of 0.02
 N5BA-C8
 1.5 with sigma of 0.02
 C32-C29
 1.5 with sigma of 0.02
 C29-C28
 1.5 with sigma of 0.02
 C28-C6
 1.5 with sigma of 0.02
 C32-C1A
 1.5 with sigma of 0.02
 C1A-C5BA
 1.5 with sigma of 0.02
 C5BA-C0BA
 1.5 with sigma of 0.02
 C16-C17
 1.2 with sigma of 0.04
 C16-C17
 1.3 with sigma of 0.04
 C15-C16
 1.3 with sigma of 0.04
 O38-C16
 1.45 with sigma of 0.04
 C1-C7AA
 2.5 with sigma of 0.04
 C7-C1
 2.5 with sigma of 0.04
 C32-C28
 2.5 with sigma of 0.04
 C6-C29
 2.5 with sigma of 0.04
 C0BA-C1A
 2.5 with sigma of 0.04
 C5BA-C32
 2.5 with sigma of 0.04
 C29-C0BA
 2.5 with sigma of 0.04
 C18-C4AA
 1.4 with sigma of 0.04
 C15-C4AA
 1.4 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O24) = Uanis(O22)
Uanis(O017) = Uanis(O31)
Uanis(O38) = Uanis(O20) = Uanis(O34)
Uanis(O26) = Uanis(O39) = Uanis(O40) = Uanis(O28) = Uanis(O36) = Uanis(O38) =
Uanis(O21)
Uanis(O20) = Uanis(O24) = Uanis(O21) = Uanis(O22) = Uanis(O23) = Uanis(O26) =
Uanis(O28) = Uanis(O27) = Uanis(O39) = Uanis(O38) = Uanis(O40) = Uanis(O34) =
Uanis(O36) = Uanis(O30) = Uanis(O31) = Uanis(O32) = Uanis(O33) = Uanis(O017) =
Uanis(O35)
Uiso(C17) = Uiso(C16) = Uiso(C15) = Uiso(C019) = Uiso(C18)
Uiso(C1A) = Uiso(C29)
Uiso(C5BA) = Uiso(C28)
Uiso(C6) = Uiso(C0BA)
4. Others
 Sof(C16)=Sof(O22)=Sof(O25)=Sof(O20)=Sof(O34)=Sof(O28)=Sof(O36)=Sof(O38)=
 Sof(O41)=Sof(O29)=Sof(O31)=Sof(O2)=Sof(C4AA)=1-FVAR(1)
 Sof(O26)=Sof(O35)=Sof(O39)=Sof(O40)=Sof(O24)=Sof(O23)=Sof(O32)=Sof(O27)=
 Sof(O21)=Sof(O30)=Sof(O33)=Sof(O017)=FVAR(1)
 Sof(C5BA)=Sof(C1A)=Sof(C0BA)=1-FVAR(2)
 Sof(C29)=Sof(C28)=Sof(C6)=FVAR(2)
 Fixed Sof: C18(0.75) C15(0.75) C17(0.75) O1(0.33333) N4AA(0.33333) C9BA(0.5)
 O9AA(0.33333) C3(0.33333) N5BA(0.33333) C7AA(0.33333) C8AA(0.5) C1BA(0.5)
 C8(0.33333) C9(0.33333) C1(0.33333) C7(0.33333) C2(0.5) C5(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5AA(H5AA,H5AB), C2BA(H2BA,H2BB), C0CA(H0CA,H0CB)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C1AA(H1AA), C11(H11), C6AA(H6AA), C10(H10)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              60569
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-12-10
_olex2_submission_special_instructions 'No special instructions were received'