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_4064445
_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            'C55 H39 B2 F20 N3'
_chemical_formula_weight         1143.51
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   'at N8 and B9 from difmap, others geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.840(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0952(4)
_cell_length_b                   10.0282(3)
_cell_length_c                   31.9122(9)
_cell_measurement_reflns_used    9194
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      0.88
_cell_volume                     5150.3(2)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.084
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            71703
_diffrn_reflns_theta_full        67.63
_diffrn_reflns_theta_max         67.63
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.8889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         8989
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+3.6627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                6613
_reflns_number_total             8989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200116q_si_005.cif
_cod_data_source_block           erk5329
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4064445