Titanocene(iii) complexes with 2-phosphinoaryloxide ligands for the catalytic dehydrogenation of dimethylamine borane.
Klahn, Marcus; Hollmann, Dirk; Spannenberg, Anke; Brückner, Angelika; Beweries, Torsten; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12103–12111; doi:10.1039/c5dt00275c

data_7034582
_publ_section_title
;
 Titanocene(iii) complexes with 2-phosphinoaryloxide ligands for the
 catalytic dehydrogenation of dimethylamine borane.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12103
_journal_page_last               12111
_journal_paper_doi               10.1039/c5dt00275c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C31.5 H28 O P Ti'
_chemical_formula_weight         501.41
_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
_audit_update_record
;
2015-01-08 deposited with the CCDC.
2015-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                100.246(1)
_cell_angle_beta                 94.705(1)
_cell_angle_gamma                112.776(1)
_cell_formula_units_Z            2
_cell_length_a                   8.9793(2)
_cell_length_b                   9.9618(2)
_cell_length_c                   15.3438(4)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.60
_cell_volume                     1227.96(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49888
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5645
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0368P)^2^+1.1199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                5018
_reflns_number_total             5645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00275c2.cif
_cod_data_source_block           ax0308
_cod_depositor_comments
'Adding full bibliography for 7034579--7034582.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31.50 H28 O P Ti'
_cod_database_code               7034582