2,2’-Bipyridine derived doubly BN fused bisphosphine-chalcogenides, [C5H3N(BF2){NCH2P(E)Ph2}]2 (E = O, S, Se): Tuning of structural features and photophysical studies
Mondal, Dipanjan; Sardar, Gopa; Kabra, Dinesh; Balakrishna, Maravanji Shivaramaiah; Dalton Transactions  (2022) –; doi:10.1039/D2DT00287F

data_7709959
_publ_section_title
;
 2,2&#x2019;-Bipyridine derived doubly B&#xF0AC;N fused
 bisphosphine-chalcogenides, [C5H3N(BF2){NCH2P(E)Ph2}]2 (E = O, S, Se):
 Tuning of structural features and photophysical studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00287F
_journal_year                    2022
_chemical_formula_moiety         'C36 H30 B2 F4 N4 O2 P2'
_chemical_formula_sum            'C36 H30 B2 F4 N4 O2 P2'
_chemical_formula_weight         710.20
_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
_audit_creation_date             2021-07-28
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2021-08-13 deposited with the CCDC.	2022-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                113.820(4)
_cell_angle_beta                 90.964(3)
_cell_angle_gamma                112.284(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2600(5)
_cell_length_b                   12.3283(5)
_cell_length_c                   14.7477(6)
_cell_measurement_reflns_used    11442
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      30.8390
_cell_measurement_theta_min      2.1610
_cell_volume                     1848.45(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50   16.00    --  -20.00   0.00-108.00  360
  2  \w    -69.00  19.00   0.50   16.00    --  -20.00 -72.00  36.00  176
  3  \w    -80.00  19.00   0.50   16.00    --  -20.00 -72.00-108.00  198
  4  \w    -35.00  18.00   0.50   16.00    --  -20.00 -72.00 108.00  106
  5  \w     -9.00  21.50   0.50   16.00    --  -20.00  72.00 -36.00   61
  6  \w   -110.00  70.00   0.50   16.00    --  -20.00   0.00-108.00  360
  7  \w    -69.00  19.00   0.50   16.00    --  -20.00 -72.00  36.00  176
  8  \w    -80.00  19.00   0.50   16.00    --  -20.00 -72.00-108.00  198
  9  \w    -35.00 -33.00   0.50   16.00    --  -20.00 -72.00 108.00    4
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0172771000
_diffrn_orient_matrix_UB_12      -0.0579888000
_diffrn_orient_matrix_UB_13      -0.0458546000
_diffrn_orient_matrix_UB_21      0.0165120000
_diffrn_orient_matrix_UB_22      0.0378545000
_diffrn_orient_matrix_UB_23      -0.0272648000
_diffrn_orient_matrix_UB_31      0.0591812000
_diffrn_orient_matrix_UB_32      0.0040800000
_diffrn_orient_matrix_UB_33      0.0058412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29048
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.243
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0705P)^2^+0.4792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4626
_reflns_number_total             6502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00287f2.cif
_cod_data_source_block           comp_5
_cod_original_cell_volume        1848.43(15)
_cod_database_code               7709959
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 88.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C9(H9), C10(H10), C3(H3), C32(H32), C4(H4), C23(H23),
 C36(H36), C26(H26), C35(H35), C33(H33), C22(H22), C21(H21), C34(H34), C19(H19),
  C27(H27), C20(H20), C30(H30), C28(H28), C29(H29), C17(H17), C13(H13),
 C15(H15), C14(H14), C16(H16)
;
_shelx_res_checksum              27935
_shelx_hkl_checksum              76800
_shelx_fab_checksum              56223
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.707