Partial hydrogenation of a tetranuclear titanium nitrido complex with ammonia borane.
Caballo, Jorge; González-Moreiras, Mariano; Greño, Maider; Mena, Miguel; Pérez-Redondo, Adrián; Yélamos, Carlos; Inorganic chemistry 53 (2014) 8851–8853; doi:10.1021/ic5015972

data_4340869
_publ_section_title
;
 Partial hydrogenation of a tetranuclear titanium nitrido complex with
 ammonia borane.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8851
_journal_page_last               8853
_journal_paper_doi               10.1021/ic5015972
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H61 N4 Ti4, C F3 O3 S, 3(C6 H5 F)'
_chemical_formula_sum            'C59 H76 F6 N4 O3 S Ti4'
_chemical_formula_weight         1226.9
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-04-28T17:52:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.044(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1010(10)
_cell_length_b                   19.791(2)
_cell_length_c                   27.531(3)
_cell_measurement_reflns_used    190
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     6025.1(10)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_unetI/netI     0.1356
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            110782
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.61
_exptl_absorpt_correction_T_max  1.415
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
This compound crystallized with three molecules of fluorobenzene, which were found
in the Fourier difference map, but it was not possible to get a chemical sensible
model for them, so Squeeze procedure was used to remove their contribution to the
structure factors.
;
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         13834
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2514
_reflns_number_gt                6944
_reflns_number_total             13834
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5015972_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4340868--4340869.cif.'
_cod_database_code               4340869