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_7709958
_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 P2 S2'
_chemical_formula_sum            'C36 H30 B2 F4 N4 P2 S2'
_chemical_formula_weight         742.32
_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_creation_date             2021-07-27
_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                108.367(3)
_cell_angle_beta                 96.762(3)
_cell_angle_gamma                90.049(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8004(3)
_cell_length_b                   13.4350(5)
_cell_length_c                   15.5523(4)
_cell_measurement_reflns_used    12002
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.3370
_cell_measurement_theta_min      2.3420
_cell_volume                     1731.58(10)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   10.00    --  -20.00   0.00-108.00  360
  2  \w    -85.50  19.00   0.50   10.00    --  -20.00 -72.00-108.00  209
  3  \w    -77.50  10.50   0.50   10.00    --  -20.00 -72.00  36.00  176
  4  \w    -50.50   2.00   0.50   10.00    --  -20.00  72.00-180.00  105
  5  \w     -9.00  21.50   0.50   10.00    --  -20.00  72.00 -36.00   61
  6  \w   -110.00  25.00   0.50   10.00    --  -20.00   0.00-180.00  270
  7  \w   -110.00  19.00   0.50   10.00    --  -20.00 -72.00-180.00  258
  8  \w    -68.50 -35.50   0.50   10.00    --  -20.00 -72.00 -36.00   66
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0261755000
_diffrn_orient_matrix_UB_12      -0.0120007000
_diffrn_orient_matrix_UB_13      -0.0471844000
_diffrn_orient_matrix_UB_21      0.0124965000
_diffrn_orient_matrix_UB_22      -0.0538947000
_diffrn_orient_matrix_UB_23      -0.0065324000
_diffrn_orient_matrix_UB_31      -0.0758730000
_diffrn_orient_matrix_UB_32      -0.0071354000
_diffrn_orient_matrix_UB_33      0.0087539000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93362
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6106
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0397P)^2^+0.7912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4739
_reflns_number_total             6106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00287f2.cif
_cod_data_source_block           comp_6
_cod_database_code               7709958
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.952
_reflns_odcompleteness_completeness 90.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.16
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C31-C36 \\sim C31-C36A
 with sigma of 0.02
 C34-C35 \\sim C34-C35A
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 C31-C35 \\sim C31-C35A
 with sigma of 0.04
 C34-C36 \\sim C34-C36A
 with sigma of 0.04
3. Others
 Fixed Sof: H34(0.68) H34A(0.32) C36(0.68) H36(0.68) C35(0.68) H35(0.68)
 C36A(0.32) H36A(0.32) C35A(0.32) H35A(0.32)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C24(H24A,H24B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C9(H9), C23(H23), C17(H17), C30(H30),
 C19(H19), C8(H8), C16(H16), C20(H20), C26(H26), C29(H29), C13(H13), C21(H21),
 C15(H15), C22(H22), C28(H28), C14(H14), C27(H27), C32(H32), C33(H33), C34(H34),
  C34(H34A), C36(H36), C35(H35), C36A(H36A), C35A(H35A)
;
_shelx_res_checksum              60731
_shelx_hkl_checksum              22042
_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 1.934
_oxdiff_exptl_absorpt_empirical_full_min 0.816