Reactions of Topologically Related “nacnacH-CN” and “P-nacnacH-CN” Chelate Ligand Systems with HB(C6F5)2
Spannhoff, Kirsten; Rojas, Rene; Fröhlich, Roland; Kehr, Gerald; Erker, Gerhard; Organometallics 30 (2011) 2377–; doi:10.1021/om200116q

data_4064448
_publ_section_title
;
 Reactions of Topologically Related &#x201C;nacnacH-CN&#x201D; and
 &#x201C;P-nacnacH-CN&#x201D; Chelate Ligand Systems with HB(C6F5)2
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2377
_journal_paper_doi               10.1021/om200116q
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C50 H32 B F10 N3 P2'
_chemical_formula_weight         937.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'at N2 from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.833(2)
_cell_angle_beta                 105.781(4)
_cell_angle_gamma                99.151(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4591(4)
_cell_length_b                   11.6827(4)
_cell_length_c                   19.1693(9)
_cell_measurement_reflns_used    7020
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     2147.98(16)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28040
_diffrn_reflns_theta_full        67.36
_diffrn_reflns_theta_max         67.36
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.8517
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00196(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0507P)^2^+1.2514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                6595
_reflns_number_total             7444
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200116q_si_008.cif
_cod_data_source_block           erk5576
_cod_original_cell_volume        2147.98(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064448