Peri-Substituted (Ace)Naphthylphosphinoboranes. (Frustrated) Lewis Pairs
Jens Beckmann; Emanuel Hupf; Enno Lork; Stefan Mebs; Inorganic Chemistry 52 (2013) 11881–11888; doi:10.1021/ic401406k

data_4336423
_publ_contact_author_email       j.beckmann@uni-bremen.de
_publ_contact_author_name        'Jens Beckmann'
_publ_section_title
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 Peri-Substituted (Ace)Naphthylphosphinoboranes. (Frustrated) Lewis Pairs
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11881
_journal_page_last               11888
_journal_paper_doi               10.1021/ic401406k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H40 B P'
_chemical_formula_sum            'C42 H40 B P'
_chemical_formula_weight         586.52
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.568(2)
_cell_length_b                   20.405(5)
_cell_length_c                   19.616(6)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.972
_cell_measurement_theta_min      9.530
_cell_volume                     3397.2(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7789
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.60
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+1.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                4339
_reflns_number_total             5933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401406k_si_001.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        3397.2(15)
_cod_database_code               4336423
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  {H2A,H2B} of C2, {H1A,H1B} of C1, {H2AA,H2AB} of C2A, H11 of C11, {H1AA,
  H1AB} of C1A, H12 of C12, H16 of C16, H16A of C16A, H17 of C17, H17A of C17A,
  H21A of C21A, H21 of C21, H22 of C22, H22A of C22A, H23 of C23, H23A of C23A,
  H24 of C24, H24A of C24A, H25 of C25, H25A of C25A, H31 of C31, H31A of C31A,
  {H32A,H32} of C32, H33 of C33, H33A of C33A, H34 of C34, H44A of C44A, H42 of
  C42, H44 of C44, H52 of C52, H54 of C54, H42A of C42A, H35A of C35A, H35 of
  C35, H34A of C34A
 At 1.5 times of:
  {H46A,H46B,H46C} of C46, {H47A,H47B,H47C} of C47, {H58A,H58B,H58C} of C58,
  {H57A,H57B,H57C} of C57, {H56A,H56B,H56C} of C56, {H48A,H48B,H48C} of C48,
  {H47D,H47E,H47F} of C47A, {H46D,H46E,H46F} of C46A, {H48D,H48E,H48F} of C48A
2. others
 Sof(C1)=Sof(H1A)=Sof(H1B)=1-Sof(H1A)=1-Sof(H1A)=1-Sof(H1A)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=1-Sof(H1A)=1-Sof(H1A)=1-Sof(H1A)=Sof(C13)=1-Sof(H1A)=Sof(C14)=1-
 Sof(H1A)=Sof(C15)=1-Sof(H1A)=Sof(C16)=Sof(H16)=1-Sof(H1A)=1-Sof(H1A)=Sof(C17)=
 Sof(H17)=1-Sof(H1A)=1-Sof(H1A)
 Sof(C20)=1-Sof(C20A)=1-Sof(C20A)=1-Sof(C20A)=Sof(C21)=Sof(H21)=Sof(C22)=
 Sof(H22)=1-Sof(C20A)=1-Sof(C20A)=Sof(C23)=Sof(H23)=1-Sof(C20A)=1-Sof(C20A)=
 Sof(C24)=Sof(H24)=1-Sof(C20A)=1-Sof(C20A)=Sof(C25)=Sof(H25)=1-Sof(C20A)=1-
 Sof(C20A)
 Sof(C30)=1-Sof(C30A)=Sof(C31)=Sof(H31)=1-Sof(C30A)=1-Sof(C30A)=1-Sof(C30A)=
 Sof(H32)=Sof(C33)=Sof(H33)=1-Sof(C30A)=1-Sof(C30A)=Sof(C34)=Sof(H34)=1-
 Sof(C30A)=1-Sof(C30A)=Sof(C35)=Sof(H35)=1-Sof(C30A)=1-Sof(C30A)
 Sof(C41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(H48C)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-
 Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-
 Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-Sof(C42)=1-
 Sof(C42)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB), C2(H2A,H2B), C2A(H2AA,H2AB)
3.b Me refined with riding coordinates:
 C47(H47A,H47B,H47C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C16(H16), C16A(H16A), C17(H17), C17A(H17A), C21A(H21A),
 C21(H21), C22(H22), C22A(H22A), C23(H23), C23A(H23A), C24(H24), C24A(H24A),
 C25(H25), C25A(H25A), C31(H31), C31A(H31A), C32(H32A), C32(H32), C33(H33),
 C33A(H33A), C34(H34), C34A(H34A), C35(H35), C35A(H35A), C42(H42), C44(H44),
 C42A(H42A), C44A(H44A), C52(H52), C54(H54)
3.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C46A(H46D,H46E,H46F), C47A(H47D,
 H47E,H47F), C48A(H48D,H48E,H48F)
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