Functionalized 1,3-dipyrrolyl-1,3-diketone difluoroboron complexes
Shenoy, Ankitha M.; Fernandes, Premie P.; Lakshmi, Vellanki; New Journal of Chemistry 49 (2025) 3987–3996; doi:10.1039/D4NJ04611K

data_7063628
_publ_section_title
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 Functionalized 1,3-dipyrrolyl-1,3-diketone difluoroboron complexes
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_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3987
_journal_page_last               3996
_journal_paper_doi               10.1039/D4NJ04611K
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C11 H8 B F2 N3 O4'
_chemical_formula_sum            'C11 H8 B F2 N3 O4'
_chemical_formula_weight         295.01
_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   mixed
_audit_creation_date             2024-08-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-02 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                92.953(3)
_cell_angle_beta                 90.580(2)
_cell_angle_gamma                108.407(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2469(3)
_cell_length_b                   7.8596(4)
_cell_length_c                   11.2611(6)
_cell_measurement_reflns_used    2550
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.74
_cell_volume                     607.55(5)
_computing_cell_refinement       'Bruker APEX4/SAINT'
_computing_data_collection       'Bruker APEX4/SAINT'
_computing_data_reduction        'Bruker APEX4/SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      300.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 QUEST diffractometer with PHOTON II detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16095
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.096
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'i-mu-s microfocus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1451 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.8669.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             300
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0666P)^2^+0.1513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1344
_reflns_number_total             2683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04611k1.cif
_cod_data_source_block           ak_no2_180724_0m_a
_cod_depositor_comments
'Adding full bibliography for 7063627--7063628.cif.'
_cod_database_code               7063628
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim N3: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
3. Rigid body (RIGU) restrains
 N3, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4), C6(H6), C9(H9), C10(H10)
;
_shelx_res_checksum              61189
_shelx_hkl_checksum              97456
_olex2_submission_special_instructions 'No special instructions were received'