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_7122960
_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 Eu2 N Nb3 O75 P2 W15, 10.5(O)'
_chemical_formula_sum            'C5 H4 B Eu2 N Nb3 O85.5 P2 W15'
_chemical_formula_weight         4859.24
_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             2018-06-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1824(3)
_cell_length_b                   14.19070(10)
_cell_length_c                   28.1627(3)
_cell_measurement_reflns_used    26592
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.998
_cell_measurement_theta_min      3.6910
_cell_volume                     8966.46(17)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46520
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    48.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.600
_exptl_crystal_description       needle
_exptl_crystal_F_000             8476
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         8.585
_refine_diff_density_min         -6.219
_refine_diff_density_rms         0.692
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         15181
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1984P)^2^+83.2764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2595
_refine_ls_wR_factor_ref         0.2767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12743
_reflns_number_total             15181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09872g2.cif
_cod_data_source_block           zyf20171215
_cod_original_formula_sum        'C5 H4 B Eu2 N Nb3 O85.50 P2 W15'
_cod_database_code               7122960
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.053
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O62) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq, Uanis(O65) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3AA) \\sim Ueq, Uanis(O75) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O66)
\\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Fixed Sof: O6BA(0.5) O0CA(0.5) O1CA(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C5(H5)
;
_shelx_res_checksum              23668
_shelx_fab_checksum              6284
_olex2_submission_special_instructions 'No special instructions were received'