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_7702086
_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         '2(C26 H32 B N P2)'
_chemical_formula_sum            'C52 H64 B2 N2 P4'
_chemical_formula_weight         862.64
_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
_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                108.455(3)
_cell_angle_beta                 104.696(3)
_cell_angle_gamma                92.445(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3495(7)
_cell_length_b                   15.2609(11)
_cell_length_c                   16.9887(12)
_cell_measurement_temperature    150(2)
_cell_volume                     2439.8(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      149.97
_diffrn_measured_fraction_theta_full 0.9919
_diffrn_measured_fraction_theta_max 0.9919
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41010
_diffrn_reflns_theta_full        27.5187
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0627 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.9328.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.1741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             921.1055
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4557
_refine_diff_density_min         -0.3692
_refine_diff_density_rms         0.0561
_refine_ls_d_res_high            0.7691
_refine_ls_d_res_low             15.4613
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    104
_refine_ls_number_parameters     564
_refine_ls_number_reflns         11157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0420
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0491P)^2^+1.0718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                9542
_reflns_number_total             11157
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt01659f2.cif
_cod_data_source_block           lf025_0m
_cod_database_code               7702086
_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:
 C17(H17), C20(H20), C41(H41), C47(H47)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C39(H39), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C52(H52)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C48(H48a,H48b,H48c), C80(H80a,
 H80b,H80c)
;
_olex2_submission_special_instructions 'No special instructions were received'