Carbon-nitrogen bond construction and carbon-oxygen double bond cleavage on a molecular titanium oxonitride: a combined experimental and computational study.
Carbó, Jorge J; García-López, Diego; González-Del Moral, Octavio; Martín, Avelino; Mena, Miguel; Santamaría, Cristina; Inorganic chemistry 54 (2015) 9401–9412; doi:10.1021/acs.inorgchem.5b00943

data_4346208
_publ_section_title
;
 Carbon-nitrogen bond construction and carbon-oxygen double bond cleavage
 on a molecular titanium oxonitride: a combined experimental and
 computational study.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9401
_journal_page_last               9412
_journal_paper_doi               10.1021/acs.inorgchem.5b00943
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H57 N1 O4 Ti3'
_chemical_formula_sum            'C44 H57 N O4 Ti3'
_chemical_formula_weight         807.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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             2012-11-19T15:39:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 121.825(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.857(2)
_cell_length_b                   21.714(5)
_cell_length_c                   17.775(4)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     4216.3(17)
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_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  0.114
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77938
_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        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_correction_T_min  0.803
_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    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.132
_refine_ls_R_factor_gt           0.0875
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+18.9896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.188
_refine_ls_wR_factor_ref         0.2125
_reflns_number_gt                6608
_reflns_number_total             9549
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b00943_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        4216.3(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H57 N1 O4 Ti3'
_cod_database_code               4346208