Boron diamide derivatives containing N-N and N-P molecular fragments.
Major, Christopher J.; Chen, Shi-Ming; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2159–2166; doi:10.1039/d3dt03665k

data_7714859
_publ_section_title
;
 Boron diamide derivatives containing N-N and N-P molecular fragments.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2159
_journal_page_last               2166
_journal_paper_doi               10.1039/d3dt03665k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H38 B N5'
_chemical_formula_sum            'C26 H38 B N5'
_chemical_formula_weight         431.42
_chemical_name_systematic        Monoclinic
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_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     iterative
_audit_creation_date             2023-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2023-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.397(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.362(2)
_cell_length_b                   6.6968(11)
_cell_length_c                   39.001(8)
_cell_measurement_reflns_used    8492
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.36
_cell_volume                     2683.8(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            45211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.669
_diffrn_reflns_theta_min         1.052
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6671
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0849 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.8950.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       Block
_exptl_crystal_F_000             936
_exptl_crystal_preparation       Metathesis
_exptl_crystal_recrystallization_method Cooling
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0312P)^2^+2.4812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4004
_reflns_number_total             5635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03665k2.cif
_cod_data_source_block           final_monoclinic_p21c_b
_cod_depositor_comments
;
Adding full bibliography for 7714859--7714862.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C104 H152 B4 N20'
_cod_original_formula_weight         1725.69
_cod_original_formula_moiety         '4(C26 H38 B N5)'
_cod_original_formula_units_Z            1
_cod_database_code               7714859
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C9(H9), C21(H21), C12(H12), C24(H24)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C23(H23A,H23B,H23C), C10(H10A,H10B,H10C), C26(H26A,H26B,H26C), C25(H25A,
 H25B,H25C)
;
_shelx_res_checksum              12776
_olex2_exptl_crystal_mounting_method Loop
_olex2_submission_special_instructions 'No special instructions were received'