Blue Emissive Amidinate Based Tetra coordinate Boron Compounds
Kannan, Ramkumar; Nayak, Prakash; Arumugam, Ramar; Krishna Rao, D.; Mote, Kaustubh R.; Murali, Anna Chandrasekar; Venkatasubbaiah, Krishnan; Chandrasekhar, Vadapalli; Dalton Transactions  (2023) –; doi:10.1039/D3DT03378C

data_7714268
_publ_section_title
;
 Blue Emissive Amidinate Based Tetra coordinate Boron Compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03378C
_journal_year                    2023
_chemical_formula_moiety         'C25 H27 B F2 N2, 0.25[C7H8], 0.25[C4H10O]'
_chemical_formula_sum            'C25 H27 B F2 N2'
_chemical_formula_weight         808.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2g0bvp
_audit_creation_date             2023-03-21
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2023-05-22 deposited with the CCDC.	2023-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.579(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.460(2)
_cell_length_b                   8.6052(8)
_cell_length_c                   24.688(3)
_cell_measurement_reflns_used    2509
_cell_measurement_temperature    298
_cell_measurement_theta_max      21.4350
_cell_measurement_theta_min      3.1390
_cell_volume                     5051.2(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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_environment      air
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.831
_diffrn_measured_fraction_theta_max 0.831
_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    -34.00  -9.00   0.50   47.21    --   10.80 -42.00 138.00   50
  2  \w     18.00  44.00   0.50   47.21    --   10.80  42.00 -68.00   52
  3  \w     13.00  38.00   0.50   47.21    --  -11.40  42.00 -68.00   50
  4  \w    -61.00 -36.00   0.50   47.21    --  -11.40 -42.00 138.00   50
  5  \w    -31.00  28.00   0.50   47.21    --   10.80  38.00  30.00  118
  6  \w     42.00  67.00   0.50   47.21    --   10.80  57.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0213571000
_diffrn_orient_matrix_UB_12      -0.0359706000
_diffrn_orient_matrix_UB_13      0.0206609000
_diffrn_orient_matrix_UB_21      -0.0205233000
_diffrn_orient_matrix_UB_22      -0.0251258000
_diffrn_orient_matrix_UB_23      0.0141185000
_diffrn_orient_matrix_UB_31      -0.0035602000
_diffrn_orient_matrix_UB_32      -0.0697874000
_diffrn_orient_matrix_UB_33      -0.0157285000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.1213
_diffrn_reflns_Laue_measured_fraction_full 0.831
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21426
_diffrn_reflns_point_group_measured_fraction_full 0.831
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.570
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         7689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0990P)^2^+0.3611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4031
_reflns_number_total             7689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03378c2.cif
_cod_data_source_block           vc1001
_cod_depositor_comments
;

2024-10-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H54 B2 F4 N4'
_cod_original_formula_weight         808.59
_cod_original_formula_moiety       '2(C25 H27 B F2 N2), 0.5[C7H8], 0.5[C4H10O]'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        5051.3(9)
_cod_database_code               7714268
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNBF
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.986
_reflns_odcompleteness_completeness 75.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00R(H00R), C00U(H00U), C00Z(H00Z), C010(H010), C011(H011), C013(H013),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A), C01B(H01B)
2.b Idealised Me refined as rotating group:
 C01C(H01C,H01D,H01E), C01D(H01U,H01V,H01W), C01E(H01F,H01G,H01H), C01G(H01I,
 H01J,H01K), C01H(H01X,H01Y,H), C01I(H01L,H01M,H01N), C01J(H01Z,HA,HB),
 C01K(H01O,H01P,H01Q), C01L(H01,HC,HD), C01M(H0AA,HE,HF), C01N(H1AA,HG,HH),
 C01O(H01R,H01S,H01T)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74613
_shelx_fab_checksum              10890
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.813