Borinine-FLP ring expansion: isolation of eight-membered B–P rings bridged by μ2 chalcogenide and chloronium ions
Frey, Nathan C.; Sarkar, Samir Kumar; Dickie, Diane A.; Molino, Andrew; Gilliard, Robert J.; Chemical Science 16 (2025) 10857–10866; doi:10.1039/D5SC02000J

data_1574615
_publ_section_title
;
 Borinine-FLP ring expansion: isolation of eight-membered B--P rings
 bridged by \m2 chalcogenide and chloronium ions
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              10857
_journal_page_last               10866
_journal_paper_doi               10.1039/D5SC02000J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C138 H97 B4 Cl2 F13 N2 O8 P4 S4'
_chemical_formula_weight         2524.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2024-07-06 deposited with the CCDC.	2025-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                74.7920(10)
_cell_angle_beta                 71.2440(10)
_cell_angle_gamma                63.3670(10)
_cell_formula_units_Z            1
_cell_length_a                   12.9579(4)
_cell_length_b                   14.3772(5)
_cell_length_c                   18.4440(7)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      30.4384
_cell_measurement_theta_min      2.6095
_cell_volume                     2879.91(18)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.15'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1365)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS double bounce multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102919
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.608
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         17551
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0751P)^2^+1.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14057
_reflns_number_total             17551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02000j2.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1574608--1574615.cif.
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_cod_database_code               1574615
_shelx_res_checksum              30710