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_7709956
_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, C H2 Cl2'
_chemical_formula_sum            'C37 H32 B2 Cl2 F4 N4 P2 S2'
_chemical_formula_weight         827.24
_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     direct
_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                108.010(7)
_cell_angle_beta                 103.978(7)
_cell_angle_gamma                92.449(6)
_cell_formula_units_Z            2
_cell_length_a                   9.3602(7)
_cell_length_b                   13.5014(9)
_cell_length_c                   16.0901(16)
_cell_measurement_reflns_used    4453
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.5100
_cell_measurement_theta_min      3.0480
_cell_volume                     1861.3(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.976
_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   -164.00 -11.00   1.00   16.00    -- -101.00   0.00-180.00  153
  2  \w   -122.00  40.00   1.00   16.00    --  -32.00   0.00  36.00  162
  3  \w   -135.00 -11.00   1.00   16.00    -- -101.00  72.00 -36.00  124
  4  \w   -106.00 -22.00   1.00   16.00    -- -101.00  72.00 144.00   84
  5  \w   -100.00 -23.00   1.00   16.00    -- -101.00  72.00  36.00   77
  6  \w   -180.00 -89.00   1.00   16.00    -- -101.00 -72.00   0.00   91
  7  \w    -97.00 -21.00   1.00   16.00    -- -101.00  72.00-180.00   76
  8  \w    -66.00 -12.00   1.00   16.00    --  -32.00  72.00-108.00   54
  9  \w   -122.00 -33.00   1.00   16.00    -- -101.00  43.00 -36.00   89
 10  \w    -95.00 -15.00   1.00   16.00    -- -101.00  72.00  72.00   80
 11  \w    -64.00 -14.00   1.00   16.00    --  -32.00  72.00  72.00   50
 12  \w   -113.00 -80.00   1.00   16.00    -- -101.00  72.00-108.00   33
 13  \w   -100.00 -29.00   1.00   16.00    -- -101.00  72.00 108.00   71
 14  \w   -106.00 -76.00   1.00   16.00    -- -101.00  72.00 -72.00   30
 15  \w   -107.00 -77.00   1.00   16.00    -- -101.00  72.00   0.00   30
 16  \w   -106.00 -76.00   1.00   16.00    -- -101.00  72.00-144.00   30
 17  \w   -191.00 -67.00   1.00   16.00    -- -101.00 -72.00  72.00  124
 18  \w   -191.00 -67.00   1.00   16.00    -- -101.00 -72.00 144.00  124
 19  \w   -191.00 -67.00   1.00   16.00    -- -101.00 -72.00-144.00  124
 20  \w   -122.00  58.00   1.00   16.00    --  -32.00   0.00 -36.00  180
 21  \w   -191.00-104.00   1.00   16.00    -- -101.00 -72.00 -36.00   87
;
_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      -0.0937631000
_diffrn_orient_matrix_UB_12      -0.1087619000
_diffrn_orient_matrix_UB_13      -0.0427337000
_diffrn_orient_matrix_UB_21      -0.0136976000
_diffrn_orient_matrix_UB_22      0.0030684000
_diffrn_orient_matrix_UB_23      0.0942479000
_diffrn_orient_matrix_UB_31      -0.1423414000
_diffrn_orient_matrix_UB_32      0.0528596000
_diffrn_orient_matrix_UB_33      -0.0145822000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1264
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23924
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.996
_diffrn_reflns_theta_min         2.998
_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    3.900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60414
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.1065
_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^)+(0.1744P)^2^+5.4978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2824
_refine_ls_wR_factor_ref         0.3303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4256
_reflns_number_total             6771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00287f2.cif
_cod_data_source_block           comp-6-CH2Cl2
_cod_database_code               7709956
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.689
_reflns_odcompleteness_completeness 96.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.83
_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:
 C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C4(H4), C15(H15), C19(H19), C23(H23), C8(H8), C10(H10),
 C9(H9), C14(H14), C5(H5), C20(H20), C21(H21), C26(H26), C32(H32), C16(H16),
 C35(H35), C34(H34), C33(H33), C13(H13), C30(H30), C22(H22), C36(H36), C29(H29),
  C27(H27), C28(H28)
;
_shelx_res_checksum              37481
_shelx_hkl_checksum              20547
_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 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.517