Optimised syntheses and purifications of 3-aryl/heterocyclic dihydrobis- and hydrotris-(pyrazolyl)borate ligands as their alkali salts
Thomas, Jarrod R.; Mifsud, Jonathan T.; Sulway, Scott A.; RSC Advances 14 (2024) 30713–30718; doi:10.1039/D4RA05723F

data_7249398
_publ_section_title
;
 Optimised syntheses and purifications of 3-aryl/heterocyclic dihydrobis-
 and hydrotris-(pyrazolyl)borate ligands as their alkali salts
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              30713
_journal_page_last               30718
_journal_paper_doi               10.1039/D4RA05723F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C32 H28 B2 Li2 N12'
_chemical_formula_sum            'C32 H28 B2 Li2 N12'
_chemical_formula_weight         616.16
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-22 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.567(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5827(5)
_cell_length_b                   21.2856(11)
_cell_length_c                   14.6160(6)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.886
_cell_measurement_theta_min      2.207
_cell_volume                     3186.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72157
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.395
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1475 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.9157.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0793P)^2^+4.6413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             3249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra05723f2.cif
_cod_data_source_block           jrt248_230907_0ma_a
_cod_database_code               7249398
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C16(0.5) H16(0.5) C13(0.5) H13(0.5) C15(0.5) H15(0.5) C14(0.5)
 H14(0.5) C10(0.6667) H10(0.6667) C9(0.6667) H9(0.6667) C9A(0.3333) H9A(0.3333)
 C10A(0.3333) H10A(0.3333) C15A(0.5) H15A(0.5) C14A(0.5) H14A(0.5) C13A(0.5)
 H13A(0.5) C16A(0.5) H16A(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C7(H7), C1(H1), C5(H5), C6(H6), C16(H16), C13(H13), C15(H15),
 C14(H14), C10(H10), C9(H9), C9A(H9A), C10A(H10A), C15A(H15A), C14A(H14A),
 C13A(H13A), C16A(H16A)
;
_shelx_res_checksum              12732
_olex2_submission_special_instructions 'No special instructions were received'