Structural elucidation of a mononuclear titanium methylidene.
Grant, Lauren N.; Ahn, Seihwan; Manor, Brian C.; Baik, Mu-Hyun; Mindiola, Daniel J.; Chemical communications (Cambridge, England) 53 (2017) 3415–3417; doi:10.1039/c7cc00654c

data_7119689
_publ_section_title
;
 Structural elucidation of a mononuclear titanium methylidene.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3415
_journal_page_last               3417
_journal_paper_doi               10.1039/c7cc00654c
_journal_volume                  53
_journal_year                    2017
_chemical_formula_sum            'C50 H77 N2 P2 Ti'
_chemical_formula_weight         815.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-06 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                79.409(2)
_cell_angle_beta                 86.348(2)
_cell_angle_gamma                75.6650(10)
_cell_formula_units_Z            4
_cell_length_a                   12.3342(3)
_cell_length_b                   14.2207(4)
_cell_length_c                   28.9433(8)
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.21
_cell_volume                     4833.9(2)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0896
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            291247
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         21616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+5.3548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                16026
_reflns_number_total             21616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00654c2.cif
_cod_data_source_block           UP9146
_cod_depositor_comments
'Adding full bibliography for 7119689--7119690.cif.'
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               7119689