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_4336424
_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         'C40 H38 B P'
_chemical_formula_sum            'C40 H38 B P'
_chemical_formula_weight         560.48
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:22:26, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.073(4)
_cell_length_b                   27.770(6)
_cell_length_c                   11.379(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.054
_cell_measurement_theta_min      4.601
_cell_volume                     3170.4(15)
_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
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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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8917
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.9
_exptl_crystal_size_min          0.9
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+1.4909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                5544
_reflns_number_total             7238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401406k_si_002.cif
_cod_data_source_block           compound1
_cod_database_code               4336424
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H25 of C25, H31 of C31, H32 of C32, H33 of C33, H34 of C34, H35 of C35, H42
  of C42, H44 of C44, H52 of C52, H54 of C54, H11 of C11, H12 of C12, H13 of
  C13, H15 of C15, H16 of C16, H17 of C17, H21 of C21, H22 of C22, H23 of C23,
  H24 of C24
 At 1.5 times of:
  {H46A,H46B,H46C} of C46, {H47A,H47B,H47C} of C47, {H48A,H48B,H48C} of C48,
  {H58A,H58B,H58C} of C58, {H57A,H57B,H57C} of C57, {H56A,H56B,H56C} of C56
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C42(H42), C44(H44), C52(H52), C54(H54)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
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