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_7709955
_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 H32 N4 O2 P2'
_chemical_formula_sum            'C36 H32 N4 O2 P2'
_chemical_formula_weight         614.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 90.335(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2473(6)
_cell_length_b                   14.8930(5)
_cell_length_c                   10.3914(4)
_cell_measurement_reflns_used    9026
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.7450
_cell_measurement_theta_min      2.1440
_cell_volume                     2978.64(18)
_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
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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      150.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -59.50   4.50   0.50   10.00    --  -20.00 -72.00-180.00  128
;
_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      -0.0088171000
_diffrn_orient_matrix_UB_12      -0.0170772000
_diffrn_orient_matrix_UB_13      -0.0616820000
_diffrn_orient_matrix_UB_21      -0.0356867000
_diffrn_orient_matrix_UB_22      0.0073559000
_diffrn_orient_matrix_UB_23      0.0129603000
_diffrn_orient_matrix_UB_31      0.0025442000
_diffrn_orient_matrix_UB_32      0.0438590000
_diffrn_orient_matrix_UB_33      -0.0261864000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            15831
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.116
_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    0.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49714
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0468P)^2^+1.6468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5115
_reflns_number_total             6484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00287f2.cif
_cod_data_source_block           comp_2
_cod_database_code               7709955
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.971
_reflns_odcompleteness_completeness 89.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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:
 N4(H4), N3(H3), C8(H8), C5(H5), C10(H10), C9(H9), C4(H4A), C17(H17), C3(H3A),
 C32(H32), C15(H15), C36(H36), C16(H16), C21(H21), C35(H35), C14(H14), C19(H19),
  C23(H23), C13(H13), C22(H22), C20(H20), C33(H33), C34(H34), C29(H29),
 C30(H30), C27(H27), C28(H28), C26(H26)
;
_shelx_res_checksum              39462
_shelx_hkl_checksum              25977
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.745