Bis(diiminate)-based boron difluoro complexes: effective synthon for bis(borenium) cations.
Parveen, Darakshan; Yadav, Rahul Kumar; Mondal, Bijan; Dallon, Marie; Sarazin, Yann; Roy, Dipak Kumar; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14139–14143; doi:10.1039/d4dt02050b

data_7716975
_publ_section_title
;
 Bis(diiminate)-based boron difluoro complexes: effective synthon for
 bis(borenium) cations.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14139
_journal_page_last               14143
_journal_paper_doi               10.1039/d4dt02050b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H52 B2 F4 N4'
_chemical_formula_sum            'C36 H52 B2 F4 N4'
_chemical_formula_weight         638.43
_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             2023-03-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-04-06 deposited with the CCDC.	2024-08-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.606(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6320(7)
_cell_length_b                   14.7782(7)
_cell_length_c                   10.9398(7)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0070
_cell_measurement_theta_min      3.5200
_cell_volume                     1771.52(19)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -48.00  -6.00   1.00   18.00    --   17.86 -53.00  49.00   42
  2  \w     -3.00  87.00   1.00   18.00    --   17.86  53.00-166.00   90
  3  \w     14.00  39.00   1.00   18.00    --   17.86 -53.00  49.00   25
  4  \w    -19.00   6.00   1.00   18.00    --  -19.11  53.00-166.00   25
  5  \w     39.00  65.00   1.00   18.00    --   17.86 178.00  90.00   26
  6  \w    -19.00  60.00   1.00   18.00    --   17.86 -99.00  30.00   79
  7  \w    -10.00  88.00   1.00   18.00    --   17.86  77.00 -90.00   98
  8  \w      9.00  35.00   1.00   18.00    --   17.86  57.00  90.00   26
  9  \w    -18.00  57.00   1.00   18.00    --   17.86 -99.00-150.00   75
 10  \w     13.00  38.00   1.00   18.00    --   17.86 -99.00 -60.00   25
 11  \w    -23.00  11.00   1.00   18.00    --  -19.11 -77.00  30.00   34
 12  \w    -79.00 -31.00   1.00   18.00    --  -19.11 -57.00  30.00   48
 13  \w    -29.00  42.00   1.00   18.00    --  -19.11  77.00 120.00   71
 14  \w    -68.00 -43.00   1.00   18.00    --  -19.11 -53.00  49.00   25
;
_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      0.0182389000
_diffrn_orient_matrix_UB_12      -0.0128236000
_diffrn_orient_matrix_UB_13      -0.0532343000
_diffrn_orient_matrix_UB_21      0.0614068000
_diffrn_orient_matrix_UB_22      0.0106925000
_diffrn_orient_matrix_UB_23      0.0364343000
_diffrn_orient_matrix_UB_31      0.0093829000
_diffrn_orient_matrix_UB_32      -0.0450173000
_diffrn_orient_matrix_UB_33      0.0238252000
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19815
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.325
_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    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       cube
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0636P)^2^+0.4405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2097
_reflns_number_total             3116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02050b2.cif
_cod_data_source_block           red1
_cod_database_code               7716975
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H52 B2 F4 N4'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C14(H14), C18(H18)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C11(H11)
2.d Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C6(H6a,H6b,H6c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c),
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c)
;
_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 2.839
_oxdiff_exptl_absorpt_empirical_full_min 0.422