Hydride Ion Abstraction from Titanocene Cyclic Organohydroborates, Cp2Ti{(μ-H)2BR2} (R2= C4H8, C5H10, C8H14), as a Function of Solvent
Plečnik, Christine E.; Liu, Fu-Chen; Liu, Shengming; Liu, Jianping; Meyers, Edward A.; Shore, Sheldon G.; Organometallics 20 (2001) 3599–; doi:10.1021/om010267m

data_4077338
_publ_section_title
;
 Hydride Ion Abstraction from Titanocene Cyclic Organohydroborates,
 Cp2Ti{(\m-H)2BR2} (R2= C4H8, C5H10, C8H14), as a Function of Solvent
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3599
_journal_paper_doi               10.1021/om010267m
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C36 H31 B F15 O2 Ti'
_chemical_formula_weight         839.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   14.8789(10)
_cell_length_b                   52.512(2)
_cell_length_c                   14.9146(10)
_cell_measurement_reflns_used    '10 frames'
_cell_measurement_temperature    193(2)
_cell_volume                     10574.1(14)
_computing_cell_refinement       'DENZO (Otwinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega at 55/-55'
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            61834
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.8976
_exptl_absorpt_correction_T_min  0.8766
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             5100
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1624
_refine_ls_number_reflns         18594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+8.6654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1799
_reflns_number_gt                11174
_reflns_number_total             18594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010267m.cif
_cod_data_source_block           '[Cp2Ti(OEt2)2][HB(C6F5)3]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C108 H93 B3 F45 O6 Ti3'
_cod_original_formula_weight         2517.95
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10574.1(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077338