Boron-Centered Compounds: Exploring the Optical Properties of Spiro Derivatives with Imidazo[1,5-<i>a</i>]Pyridines.
Cinco, Anita; Ardizzoia, G. Attilio; Brenna, Stefano; Therrien, Bruno; Colombo, Gioele; Molecules (Basel, Switzerland) 30 (2025) 2552–; doi:10.3390/molecules30122552

data_1575065
_publ_section_title
;
 Boron-Centered Compounds: Exploring the Optical Properties of Spiro
 Derivatives with Imidazo[1,5-<i>a</i>]Pyridines.
;
_journal_issue                   12
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              2552
_journal_paper_doi               10.3390/molecules30122552
_journal_volume                  30
_journal_year                    2025
_chemical_formula_moiety         'C26 H19 B N2 O, 1(H2O)'
_chemical_formula_sum            'C26 H21 B N2 O2'
_chemical_formula_weight         404.293
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_symmetry_Int_Tables_number      88
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.6167(5)
_cell_length_b                   26.6167(5)
_cell_length_c                   11.7810(2)
_cell_measurement_reflns_used    25602
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      69.74
_cell_measurement_theta_min      7.08
_cell_volume                     8346.2(3)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.9878
_diffrn_measured_fraction_theta_max 0.9678
_diffrn_measurement_details
;
 1276 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.9878
_diffrn_reflns_Laue_measured_fraction_max 0.9678
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25358
_diffrn_reflns_point_group_measured_fraction_full 0.9878
_diffrn_reflns_point_group_measured_fraction_max 0.9678
_diffrn_reflns_theta_full        67.6859
_diffrn_reflns_theta_max         69.74
_diffrn_reflns_theta_min         7.08
_diffrn_source                   'Primux 100 micro'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.8069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3402.863
_exptl_crystal_recrystallization_method
'crystallized by slow evaporation of diethylether in DCM'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.1482
_refine_diff_density_min         -0.1643
_refine_diff_density_rms         0.0328
_refine_ls_d_res_high            0.8218
_refine_ls_d_res_low             6.2555
_refine_ls_goodness_of_fit_ref   1.0536
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.0077
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+2.5241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              0
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                3346
_reflns_number_total             3814
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Compound3a.cif
_cod_data_source_block           compound3a
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C26 H21 B1 N2 O2'
_cod_database_code               1575065
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25)
3.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 652\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O] per Formula Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'mounted on loop with oil'
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   5.0
_stoe_evaluation_integration_b   -0.5
_stoe_evaluation_integration_ems 0.016
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 96.9
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 139.5
_stoe_evaluation_lana_max_2theta_desired 139.5
_stoe_evaluation_lana_mean_redundancy 5.0
_stoe_evaluation_lana_number_refls_after_or 19120
_stoe_evaluation_lana_number_refls_outliers 6238
_stoe_evaluation_lana_number_refls_total 25358
_stoe_evaluation_lana_number_refls_unique 3814
_stoe_evaluation_lana_number_refls_written 25358
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 4/m
_stoe_evaluation_lana_table
;
----------------------------------------------------------------------------
2Theta          20.8   34.8   48.8   62.8   76.8   90.8  104.8  118.8  132.8
----------------------------------------------------------------------------
<Resolution>    4.02   2.53   1.86   1.48   1.24   1.08   0.97   0.90   0.85
N(total)         422   1463   2225   2811   5739   3912   3787   3170   1829
<Redundancy>     6.0    7.1    6.2    4.8    7.8    4.9    4.5    3.9    3.0
Complet. [%%]   100.0  100.0  100.0  100.0  100.0   99.8   99.6   98.5   81.6
<I/sigma>      538.8  184.8  106.3   47.7   32.1   24.8   12.3    8.1    7.3
R(int)         0.010  0.015  0.016  0.019  0.021  0.020  0.036  0.057  0.088
----------------------------------------------------------------------------
;
_stoe_measurement_identifier     GAMP40
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '6.2 s'
_stoe_measurement_min_exposure_per_frame '1.5 s'
_stoe_measurement_total_exposure_time '2.2 h'
_stoe_measurement_total_frame_number 1276
_stoe_measurement_total_run_number 14
_stoe_measurement_tube_power     '50.0 W'