Reactions of 1,1- and 1,2-bis-boranes with a protic diamine and hydrazine.
Yeung, Jason; Yeganeh-Salman, Amir; Miao, Linkun; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18727–18735; doi:10.1039/d4dt02704c

data_7717305
_publ_section_title
;
 Reactions of 1,1- and 1,2-bis-boranes with a protic diamine and
 hydrazine.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18727
_journal_page_last               18735
_journal_paper_doi               10.1039/d4dt02704c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C35 H19 B2 F20 N2 Si, 1.75[CH2Cl2]'
_chemical_formula_sum            'C36.75 H22.5 B2 Cl3.5 F20 N2 Si'
_chemical_formula_weight         1045.887
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_Int_Tables_number      29
_audit_creation_date             2024-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.84(2)
_cell_length_b                   13.348(18)
_cell_length_c                   20.36(3)
_cell_measurement_reflns_used    3422
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      21.20
_cell_measurement_theta_min      2.04
_cell_volume                     4033(10)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1560
_diffrn_reflns_av_unetI/netI     0.1607
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.9970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27007
_diffrn_reflns_point_group_measured_fraction_full 0.9913
_diffrn_reflns_point_group_measured_fraction_max 0.9913
_diffrn_reflns_theta_full        24.9998
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       block
_exptl_crystal_F_000             2086.428
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5122
_refine_diff_density_min         -0.3978
_refine_diff_density_rms         0.0873
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             9.9253
_refine_ls_extinction_coef       0.0034(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9698
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    29
_refine_ls_number_parameters     545
_refine_ls_number_reflns         7034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.9698
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0085P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.985
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              -24
_reflns_number_gt                4679
_reflns_number_total             7034
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt02704c2.cif
_cod_data_source_block           final_orthorhombic_a
_cod_depositor_comments
'Adding full bibliography for 7717302--7717308.cif.'
_cod_original_cell_volume        4035(10)
_cod_original_sg_symbol_Hall     ' P 2c -2ac'
_cod_original_formula_sum        'C36.75 H22.5 B2 Cl3.5 F20 N2 Si1'
_cod_database_code               7717305
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N00M(H00a,H00b), N00N(H00c,H00d), C00O(H00e,H00f)
2.b Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C014(H014), C019(H019), C01B(H01B)
2.c Idealised Me refined as rotating group:
 C00W(H00g,H00h,H00i), C01C(H01a,H01c,H01d), C01D(H01e,H01f,H01g)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 288 electrons were 
found in a volume of 860\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.75[CH2Cl2] per Asymmetric Unit 
which account for 294 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'