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_7709960
_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_absolute_configuration unk
_chemical_formula_moiety         'C36 H32 N4 P2 Se2'
_chemical_formula_sum            'C36 H32 N4 P2 Se2'
_chemical_formula_weight         740.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 117.871(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4030(6)
_cell_length_b                   18.0437(4)
_cell_length_c                   20.5579(5)
_cell_measurement_reflns_used    43810
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.0470
_cell_measurement_theta_min      1.6770
_cell_volume                     6690.4(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 1.171.40.15 (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 1.000
_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    -91.00  49.00   0.50    8.00    --  -20.00   0.00-108.00  280
  2  \w    -45.00 -14.00   0.50    8.00    --  -20.00  72.00-180.00   62
  3  \w   -110.00  -9.50   0.50    8.00    --  -20.00   0.00-180.00  201
  4  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00-180.00  360
  5  \w    -32.00   2.50   0.50    8.00    --  -20.00 -72.00 108.00   69
  6  \w   -110.00 -61.00   0.50    8.00    --  -20.00   0.00  36.00   98
;
_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      0.0304470000
_diffrn_orient_matrix_UB_12      0.0232475000
_diffrn_orient_matrix_UB_13      0.0219687000
_diffrn_orient_matrix_UB_21      -0.0084701000
_diffrn_orient_matrix_UB_22      -0.0035757000
_diffrn_orient_matrix_UB_23      0.0295988000
_diffrn_orient_matrix_UB_31      0.0234141000
_diffrn_orient_matrix_UB_32      -0.0315088000
_diffrn_orient_matrix_UB_33      0.0128229000
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68419
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.619
_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    2.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27984
_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    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 8101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1585
_refine_ls_number_reflns         22821
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0458P)^2^+4.1323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                20483
_reflns_number_total             22821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00287f2.cif
_cod_data_source_block           comp_4
_cod_database_code               7709960
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C36H28N4P2Se2
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.470
_reflns_odcompleteness_completeness 89.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.12
_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:
 C96(H96A,H96B), C11(H11C,H11D), C119(H11A,H11B), C83(H83A,H83B), C60(H60A,
 H60B), C47(H47A,H47B), C24(H24A,H24B), C132(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 N12(H12), N4(H4), N14(H14), N3(H3), N6(H6), N10(H10), N16(H16), N8(H8),
 C3(H3A), C80(H80), C41(H41), C39(H39), C5(H5), C131(H131), C53(H53), C69(H69),
 C36(H36), C111(H111), C72(H72), C118(H118), C40(H40), C21(H21), C82(H82),
 C46(H46), C92(H92), C59(H59), C98(H98), C35(H35), C44(H44), C45(H45), C70(H70),
  C71(H71), C130(H130), C134(H134), C75(H75), C117(H117), C8(H8A), C68(H68),
 C81(H81), C10(H10A), C22(H22), C34(H34), C104(H104), C121(H121), C108(H108),
 C4(H4A), C15(H15), C23(H23), C77(H77), C9(H9), C20(H20), C32(H32), C107(H107),
 C76(H76), C112(H112), C99(H99), C87(H87), C116(H116), C113(H113), C88(H88),
 C52(H52), C19(H19), C89(H89), C100(H100), C57(H57), C123(H123), C51(H51),
 C102(H102), C49(H49), C26(H26), C66(H66), C86(H86), C50(H50), C125(H125),
 C91(H91), C127(H127), C13(H13), C55(H55), C136(H136), C85(H85), C122(H122),
 C58(H58), C135(H135), C106(H106), C28(H28), C105(H105), C129(H129), C101(H101),
  C95(H95), C141(H141), C124(H124), C17(H17), C33(H33), C30(H30), C64(H64),
 C138(H138), C144(H144), C65(H65), C27(H27), C140(H140), C62(H62), C128(H128),
 C93(H93), C94(H94), C137(H137), C63(H63), C14(H14A), C56(H56), C16(H16A),
 C29(H29), C143(H143), C142(H142)
;
_shelx_res_checksum              30248
_shelx_hkl_checksum              24157
_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 4.601
_oxdiff_exptl_absorpt_empirical_full_min 0.772