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_7702081
_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 H38 B N P2'
_chemical_formula_sum            'C26 H38 B N P2'
_chemical_formula_weight         437.37
_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             2015-11-07
_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                 91.698(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9183(5)
_cell_length_b                   16.6266(8)
_cell_length_c                   17.4581(10)
_cell_measurement_temperature    150(2)
_cell_volume                     2587.6(2)
_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      149.7
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43224
_diffrn_reflns_theta_full        27.5631
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0535 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.9690.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.1226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             945.1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5015
_refine_diff_density_min         -0.3181
_refine_diff_density_rms         0.0734
_refine_ls_d_res_high            0.7680
_refine_ls_d_res_low             12.0375
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0420
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0498P)^2^+1.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -9
_reflns_number_gt                4443
_reflns_number_total             5962
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt01659f2.cif
_cod_data_source_block           LF002_0ma
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7702081
_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. Others
 Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22c)=Sof(H22d)=
 Sof(C23A)=Sof(H23c)=Sof(H23d)=Sof(C24A)=Sof(H24c)=Sof(H24d)=Sof(C25A)=
 Sof(H25c)=Sof(H25d)=Sof(C26A)=Sof(H26c)=Sof(H26d)=1-FVAR(1)
 Sof(C19)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(C23)=
 Sof(H23a)=Sof(H23b)=Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(C25)=Sof(H25a)=Sof(H25b)=
 Sof(C26)=Sof(H26a)=Sof(H26b)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C21(H21), C21A(H21A)
3.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C22A(H22c,H22d), C23(H23a,H23b), C23A(H23c,H23d), C24(H24a,
 H24b), C24A(H24c,H24d), C25(H25a,H25b), C25A(H25c,H25d), C26(H26a,H26b),
 C26A(H26c,H26d)
3.c Me refined with riding coordinates:
 C1(H1a,H1b,H1c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'