Reactions of iodine-nitrene reagents with boranes.
Postle, Shawn; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4436–4439; doi:10.1039/c5dt00142k

data_7033906
_publ_section_title
;
 Reactions of iodine-nitrene reagents with boranes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4436
_journal_page_last               4439
_journal_paper_doi               10.1039/c5dt00142k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C31 H22 B F15 N O3 P S, C7 H8'
_chemical_formula_sum            'C38 H30 B F15 N O3 P S'
_chemical_formula_weight         907.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2014-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2014-12-28 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                83.047(3)
_cell_angle_beta                 80.953(3)
_cell_angle_gamma                87.098(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2520(4)
_cell_length_b                   13.7632(7)
_cell_length_c                   17.0976(8)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.61
_cell_volume                     1902.59(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.9889
_diffrn_measured_fraction_theta_max 0.9889
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31528
_diffrn_reflns_theta_full        27.4484
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0403 before and 0.0328 after correction.
The Ratio of minimum to maximum transmission is 0.9582.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.5839
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             921.2410
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.8200
_refine_diff_density_min         -0.4974
_refine_diff_density_rms         0.0612
_refine_ls_d_res_high            0.7709
_refine_ls_d_res_low             13.6549
_refine_ls_goodness_of_fit_ref   1.0569
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0569
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.4433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7447
_reflns_number_total             8605
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt00142k2.cif
_cod_data_source_block           sp014_0m
_cod_depositor_comments
'Adding full bibliography for 7033906--7033909.cif.'
_cod_database_code               7033906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C22-C23
 1.54 with sigma of 0.02
3. Others
 Fixed Uiso: H20(0.06) H21(0.06) H23a(0.06) H23b(0.06) H23c(0.06) H25(0.06)
 H26a(0.06) H26b(0.06) H27a(0.06) H27b(0.06) H27c(0.06) H28a(0.06) H28b(0.06)
 H29a(0.06) H29b(0.06) H29c(0.06) H30a(0.06) H30b(0.06) H31a(0.06) H31b(0.06)
 H31c(0.06) H32a(0.06) H32b(0.06) H32c(0.06) H34(0.06) H35(0.06) H36(0.06)
 H37(0.06) H38(0.06)
4.a Secondary CH2 refined with riding coordinates:
 C26(H26a,H26b), C28(H28a,H28b), C30(H30a,H30b)
4.b Me refined with riding coordinates:
 C23(H23a,H23b,H23c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C31(H31a,H31b,
 H31c)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C24(H24), C25(H25), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38)
4.d Idealised Me refined as rotating group:
 C32(H32a,H32b,H32c)
;
_olex2_submission_special_instructions 'No special instructions were received'