Boronic acid derivatized lanthanide‒polyoxometalates with novel B‒OH‒Ln and B‒O‒Nb bridges
Li, Shujun; Zhao, Yue; Qi, Huihui; Zhou, Yanfang; Liu, Shuxia; Ma, Xiaoming; Zhang, Jie; Chen, Xuenian; Chemical Communications  (2019) –; doi:10.1039/C8CC09872G

data_7122959
_publ_section_title
;
 Boronic acid derivatized lanthanide--polyoxometalates with novel
 B--OH--Ln and B--O--Nb bridges
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09872G
_journal_year                    2019
_chemical_formula_moiety
'C20 H16 B4 Er2.15 N4 Nb3 O81.05 P2 W15, Er0.85 O6.45, 17.75(O)'
_chemical_formula_sum            'C20 H16 B4 Er3 N4 Na0.5 Nb3 O104.75 P2 W15'
_chemical_formula_weight         5643.30
_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
_audit_creation_date             2018-06-01
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                72.5180(10)
_cell_angle_beta                 72.2610(10)
_cell_angle_gamma                87.635(2)
_cell_formula_units_Z            2
_cell_length_a                   17.8960(3)
_cell_length_b                   18.9430(3)
_cell_length_c                   18.9630(3)
_cell_measurement_reflns_used    28660
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.8460
_cell_measurement_theta_min      4.0500
_cell_volume                     5831.13(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -70.00  30.00   0.25    1.00    --    0.00 -77.00  60.00  400
  2  \w    -21.00  69.00   0.25    1.00    --    0.00  57.00-180.00  360
  3  \w    -21.00  69.00   0.25    1.00    --    0.00  57.00-120.00  360
  4  \w   -127.00 -79.00   0.25    2.00    --  -55.27 -99.00 120.00  192
  5  \w    -85.00  15.00   0.25    2.00    --  -55.27  77.00 -60.00  400
  6  \w    -77.00  14.00   0.25    2.00    --  -55.27  57.00-120.00  364
  7  \w   -127.00 -73.00   0.25    2.00    --  -55.27-125.00-150.00  216
  8  \w     34.00 124.00   0.25    2.00    --   55.27  57.00 120.00  360
  9  \w     30.00 128.00   0.25    2.00    --   55.27  38.00-180.00  392
 10  \w    -17.00  81.00   0.25    2.00    --   55.27 -38.00   0.00  392
 11  \w     23.00 113.00   0.25    2.00    --   55.27-125.00  60.00  360
 12  \w     34.00 124.00   0.25    2.00    --   55.27  57.00 150.00  360
 13  \w     40.00 132.00   0.25    7.00    --  110.54 -50.00-150.00  368
 14  \w     38.00 115.00   0.25    7.00    --  110.54-111.00-180.00  308
 15  \w     38.00 145.00   0.25    7.00    --  110.54 -25.00  60.00  428
 16  \w     39.00 149.00   0.25    7.00    --  110.54 -92.00-150.00  440
 17  \w     40.00 141.00   0.25    7.00    --  110.54 -77.00   0.00  404
 18  \w    100.00 178.00   0.25    7.00    --  110.54 111.00-180.00  312
 19  \w     89.00 178.00   0.25    7.00    --  110.54  50.00 150.00  356
 20  \w     39.00 102.00   0.25    7.00    --  110.54-111.00 120.00  252
 21  \w     61.00  87.00   0.25    7.00    --  110.54 -64.00-180.00  104
 22  \w     72.00  98.00   0.25    7.00    --  110.54 178.00  60.00  104
 23  \w     96.00 169.00   0.25    7.00    --  110.54  38.00 -60.00  292
 24  \w     39.00 139.00   0.25    7.00    --  110.54 -25.00 -30.00  400
 25  \w     38.00 112.00   0.25    7.00    --  110.54-111.00  30.00  296
 26  \w    111.00 157.00   0.25    7.00    --  110.54 111.00 -60.00  184
 27  \w     42.00 143.00   0.25    7.00    --  110.54 -25.00 120.00  404
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0217243000
_diffrn_orient_matrix_UB_12      -0.0555831000
_diffrn_orient_matrix_UB_13      0.0678749000
_diffrn_orient_matrix_UB_21      0.0578543000
_diffrn_orient_matrix_UB_22      -0.0344921000
_diffrn_orient_matrix_UB_23      -0.0575336000
_diffrn_orient_matrix_UB_31      0.0661426000
_diffrn_orient_matrix_UB_32      0.0548925000
_diffrn_orient_matrix_UB_33      -0.0095298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            54816
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.117
_diffrn_reflns_theta_min         3.470
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    33.933
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.214
_exptl_crystal_description       block
_exptl_crystal_F_000             4989
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.081
_refine_diff_density_min         -3.457
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1484
_refine_ls_number_reflns         22525
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0191P)^2^+186.7926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19983
_reflns_number_total             22525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09872g2.cif
_cod_data_source_block           pqp20170322
_cod_original_formula_sum        'C20 H16 B4 Er3 N4 Na0.50 Nb3 O104.75 P2 W15'
_cod_database_code               7122959
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'P1 W1 O1 B1 C1 N1 Nb1'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Er4-O3AA \\sim Er4-O2AA \\sim Er4-O1AA \\sim Er4-O0AA \\sim Er4-O4AA \\sim
Er4-O75 \\sim Er4-O42
 with sigma of 0.02
3. Rigid bond restraints
 O0AA, O75, O3AA, O4AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O0AA) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O2AA) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(O4AA) \\sim Ueq,
Uanis(O3AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O66L) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: Er3(0.85) O11(0.85) Er4(0.15) O17(0.75) O18(0.5) O20(0.5)
 O54F(0.85) O75O(0.85) O91T(0.85) O101(0.85) O10(0.5) O112(0.85) O113(0.85)
 O123(0.5) O3(0.5) O42(0.15) O3AA(0.5) O1AA(0.3) O2AA(0.15) O0AA(0.15)
 O75(0.15) O4AA(0.15) O1(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C14(H14), C15(H15), C16I(H16I), C17(H17), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              96223
_shelx_fab_checksum              18458
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.788