Ferrocenylhydridoborates: Synthesis, Structural Characterization, and Application to the Preparation of Ferrocenylborane Polymers
Matthias Scheibitz; Haiyan Li; Jan Schnorr; Alejandro Sánchez Perucha; Michael Bolte; Hans-Wolfram Lerner; Frieder Jäkle; Matthias Wagner; Journal of the American Chemical Society 131 (2009) 16319–16329; doi:10.1021/ja906575s

data_4105315
_publ_section_title
;
 Ferrocenylhydridoborates: Synthesis, Structural Characterization, and
 Application to the Preparation of Ferrocenylborane Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16319
_journal_page_last               16329
_journal_paper_doi               10.1021/ja906575s
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C41.33 H81.33 B4 Fe2 Li4 O5.33'
_chemical_formula_weight         846.43
_chemical_name_systematic        ?
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.324(16)
_cell_angle_beta                 92.741(16)
_cell_angle_gamma                99.274(16)
_cell_formula_units_Z            3
_cell_length_a                   14.798(3)
_cell_length_b                   15.367(3)
_cell_length_c                   17.476(4)
_cell_measurement_reflns_used    8818
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.6
_cell_volume                     3801.6(14)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1060
_diffrn_reflns_av_sigmaI/netI    0.2410
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26134
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         3.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.7587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 1990; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.667
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         13536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.667
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0011P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                5036
_reflns_number_total             13536
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja906575s_si_003.cif
_cod_data_source_block           wa291
_cod_database_code               4105315