PNPCB heterocycles via thermal and Lewis acid catalyzed trans-hydroborations.
Fan, Louie; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 9229–9234; doi:10.1039/c6dt01659f

data_7702084
_publ_section_title
;
 PNPCB heterocycles via thermal and Lewis acid catalyzed
 trans-hydroborations.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9229
_journal_page_last               9234
_journal_paper_doi               10.1039/c6dt01659f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H32 B N P2'
_chemical_formula_sum            'C26 H32 B N P2'
_chemical_formula_weight         431.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-04-25 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.777(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1910(12)
_cell_length_b                   9.0756(8)
_cell_length_c                   17.2932(13)
_cell_measurement_temperature    150(2)
_cell_volume                     2505.5(3)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149.69
_diffrn_measured_fraction_theta_full 0.9893
_diffrn_measured_fraction_theta_max 0.9893
_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  0.0915
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40452
_diffrn_reflns_theta_full        27.5249
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0746 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.9372.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             921.1055
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5310
_refine_diff_density_min         -0.4996
_refine_diff_density_rms         0.1148
_refine_ls_d_res_high            0.7690
_refine_ls_d_res_low             9.6694
_refine_ls_goodness_of_fit_ref   1.0222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0222
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.8671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -22
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -11
_reflns_number_gt                3823
_reflns_number_total             5713
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt01659f2.cif
_cod_data_source_block           LF001_0ma
_cod_original_cell_volume        2505.5(4)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7702084
_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 Ternary CH refined with riding coordinates:
 C5(H5), C2(H2)
2.b Me refined with riding coordinates:
 C4(H4a,H4b,H4c), C1(H1d,H1e,H1f), C3(H3a,H3b,H3c), C6(H6a,H6b,H6c)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C24(H24), C23(H23), C22(H22), C18(H18), C25(H25), C26(H26), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C15(H15), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'