Synthesis of tetraarylborates via tetralithio intermediates and the effect of polar functional groups and cations on their crystal structures.
Tomaszewski, Patryk; Wiszniewski, Marcin; Serwatowski, Janusz; Woźniak, Krzysztof; Durka, Krzysztof; Luliński, Sergiusz; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16627–16637; doi:10.1039/c8dt04068k

data_7047930
_publ_section_title
;
 Synthesis of tetraarylborates via tetralithio intermediates and the
 effect of polar functional groups and cations on their crystal
 structures.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16627
_journal_page_last               16637
_journal_paper_doi               10.1039/c8dt04068k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H24 B5 O8, 2(H2 O), 2(H1.50 O), H4 N'
_chemical_formula_sum            'C24 H35 B5 N O12'
_chemical_formula_weight         583.58
_chemical_melting_point          'decomposition > 340 C'
_chemical_name_systematic
;
Ammonium tetrakis[4-(dihydroxyboryl)phenyl]borate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-09-19 deposited with the CCDC.
2018-10-31 downloaded from the CCDC.
;
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_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1966(9)
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_cell_length_c                   11.9968(16)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    100(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
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(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.608
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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.608
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_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2573
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_diffrn_reflns_point_group_measured_fraction_max 0.734
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.386
_diffrn_reflns_theta_min         4.826
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.854
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_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone, water'
_exptl_crystal_size_max          0.03
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_refine_diff_density_max         0.259
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         1678
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1178P)^2^+2.6238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.399
_reflns_Friedel_fraction_full    0.269
_reflns_Friedel_fraction_max     0.446
_reflns_number_gt                1609
_reflns_number_total             1678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04068k2.cif
_cod_data_source_block           3d
_cod_depositor_comments
'Adding full bibliography for 7047930--7047932.cif.'
_cod_database_code               7047930
_shelxl_version_number           2013-4
_shelx_res_checksum              95025