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_7122961
_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         'C5 H4 B Er2 N Nb3 O75 P2 W15, 19(O)'
_chemical_formula_sum            'C5 H4 B Er2 N Nb3 O94 P2 W15'
_chemical_formula_weight         5025.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.06.29 svn.r3433 for OlexSys, GUI svn.r5356)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.388(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.0950(6)
_cell_length_b                   14.2098(4)
_cell_length_c                   28.0704(9)
_cell_measurement_reflns_used    19011
_cell_measurement_temperature    291.29(10)
_cell_measurement_theta_max      28.8960
_cell_measurement_theta_min      3.6070
_cell_volume                     8923.1(5)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.29(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_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      5.00  68.00   1.00   18.79    --   15.98   0.00  30.00   63
  2  \w     14.00  40.00   1.00   18.79    --   15.98  57.00 -60.00   26
  3  \w    -11.00  84.00   1.00   18.79    --   15.98  77.00   0.00   95
  4  \w      8.00  33.00   1.00   18.79    --   15.98  57.00 150.00   25
  5  \w    -53.00  35.00   1.00   18.79    --   15.98 -38.00-150.00   88
;
_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      -0.0128157000
_diffrn_orient_matrix_UB_12      -0.0009339000
_diffrn_orient_matrix_UB_13      -0.0257229000
_diffrn_orient_matrix_UB_21      0.0289850000
_diffrn_orient_matrix_UB_22      0.0014282000
_diffrn_orient_matrix_UB_23      -0.0043104000
_diffrn_orient_matrix_UB_31      0.0010802000
_diffrn_orient_matrix_UB_32      -0.0498805000
_diffrn_orient_matrix_UB_33      0.0003348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            55954
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         28.951
_diffrn_reflns_theta_min         3.232
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    21.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14035
_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    3.741
_exptl_crystal_description       block
_exptl_crystal_F_000             8788
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.683
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         20650
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+171.1901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16513
_reflns_number_total             20650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09872g2.cif
_cod_data_source_block           pqp-16-11-10-nb3+er+bi
_cod_database_code               7122961
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'P1 W1 Nb1 O1 '
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O13W) \\sim Ueq, Uanis(O15W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C9(H9), C10(H10), C11(H11)
;
_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 4.536
_oxdiff_exptl_absorpt_empirical_full_min 0.487