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_7041172
_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         'C28 H34 B2 Mn Mo6 N2 O28, 3(C16 H36 N)'
_chemical_formula_sum            'C76 H142 B2 Mn Mo6 N5 O28'
_chemical_formula_weight         2226.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 128.966(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.796(3)
_cell_length_b                   13.2361(3)
_cell_length_c                   25.8822(19)
_cell_measurement_reflns_used    10798
_cell_measurement_temperature    284.17(10)
_cell_measurement_theta_max      75.4090
_cell_measurement_theta_min      3.6720
_cell_volume                     9534.7(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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 0.983
_diffrn_measurement_details
;
  1 omega  -81.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9342   19.0000  120.0000 116

  2 omega  -96.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9342  125.0000 -180.0000 82

  3 omega  -46.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9342   37.0000 -180.0000 81

  4 omega  -57.00   -7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9342  125.0000  -90.0000 50

  5 omega   45.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9342 -125.0000   90.0000 41

  6 omega   74.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -77.0000 -180.0000 27

  7 omega   33.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000  120.0000 57

  8 omega   42.00   85.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000 -120.0000 43

  9 omega   86.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063   30.0000   90.0000 92

 10 omega   40.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -45.0000  150.0000 57

 11 omega   36.00  144.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -77.0000  -30.0000 108

 12 omega   84.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063 -111.0000   90.0000 27

 13 omega  114.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063   45.0000  150.0000 64

 14 omega   96.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063   79.0000  -15.0000 25

 15 omega  112.00  139.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -77.0000 -180.0000 27

 16 omega   38.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063 -111.0000  -60.0000 77

 17 omega  131.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063   79.0000  -15.0000 27

 18 omega   82.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063   61.0000   30.0000 95

 19 omega   32.00   87.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -30.0000   60.0000 55

 20 omega   41.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2063  -94.0000  150.0000 66
;
_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      0.0099407000
_diffrn_orient_matrix_UB_12      0.1128128000
_diffrn_orient_matrix_UB_13      0.0185291000
_diffrn_orient_matrix_UB_21      -0.0462732000
_diffrn_orient_matrix_UB_22      0.0277820000
_diffrn_orient_matrix_UB_23      -0.0697051000
_diffrn_orient_matrix_UB_31      -0.0287745000
_diffrn_orient_matrix_UB_32      -0.0056655000
_diffrn_orient_matrix_UB_33      0.0257381000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33269
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.635
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_F_000             4576
_refine_diff_density_max         1.661
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+39.8885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8273
_reflns_number_total             9745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04197c2.cif
_cod_data_source_block           hk-2-170-2-diol
_cod_depositor_comments
'Adding full bibliography for 7041170--7041172.cif.'
_cod_original_cell_volume        9534.8(16)
_cod_database_code               7041172
_chemical_oxdiff_formula         'C B N Mo O Mn'
_shelx_estimated_absorpt_t_max   1
_shelx_estimated_absorpt_t_min   0.66695
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Secondary CH2 refined with riding coordinates:
 C00K(H00M,H00N), C00N(H00O,H00P), C00O(H00Q,H00R), C00P(H00A,H00B), C00Q(H00S,
 H00T), C00R(H00C,H00D), C00S(H00U,H00V), C00T(H00E,H00F), C00U(H00G,H00H),
 C00V(H00I,H00J), C00X(H00W,H00X), C00Y(H00K,H00L), C00Z(H00Y,H), C011(H01A,
 H01B), C012(H01C,H01D), C014(H01E,H01F), C016(H2AA,HA), C017(H3AA,HB),
 C019(H01G,H01H), C01C(H01I,H01J), C01E(H01K,H01L), C01K(H01,HG), C01M(H0AA,HH),
  C01O(H1AA,HI)
2.b Aromatic/amide H refined with riding coordinates:
 C010(H010), C015(H015), C018(H018), C01A(H01Y), C01F(H01Z)
2.c Idealised Me refined as rotating group:
 C01D(H4AA,HC,HD), C01G(H01M,H01N,H01O), C01H(H01P,H01Q,H01R), C01I(H01S,H01T,
 H01U), C01J(H5AA,HE,HF), C01L(H01V,H01W,H01X)
;
_shelx_res_checksum              33997
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-26
_olex2_submission_special_instructions 'No special instructions were received'