Cp<sub>2</sub>Ti(κ<sup>2</sup><i>-</i><sup> <i>t</i> </sup>BuNCN<sup> <i>t</i> </sup>Bu): A Complex with an Unusual κ<sup>2</sup> Coordination Mode of a Heterocumulene Featuring a Free Carbene.
Beaumier, Evan P.; Gordon, Christopher P.; Harkins, Robin P.; McGreal, Meghan E.; Wen, Xuelan; Copéret, Christophe; Goodpaster, Jason D.; Tonks, Ian A.; Journal of the American Chemical Society 142 (2020) 8006–8018; doi:10.1021/jacs.0c02487

data_4134704
_publ_section_title
;
 Cp<sub>2</sub>Ti(\k<sup>2</sup><i>-</i><sup> <i>t</i> </sup>BuNCN<sup>
 <i>t</i> </sup>Bu): A Complex with an Unusual \k<sup>2</sup> Coordination
 Mode of a Heterocumulene Featuring a Free Carbene.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8006
_journal_page_last               8018
_journal_paper_doi               10.1021/jacs.0c02487
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         C20TiN2O3SF3H29
_chemical_formula_sum            'C20 H29 F3 N2 O3 S Ti'
_chemical_formula_weight         482.41
_chemical_name_common            Cp2TitBuNCHNtBuOTf
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.4491(11)
_cell_length_b                   16.3991(14)
_cell_length_c                   20.2594(15)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.46
_cell_measurement_theta_min      2.20
_cell_volume                     4468.3(6)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            113214
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         2.010
_diffrn_source                   fine
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       Plates
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+5.7295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5505
_reflns_number_total             6842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02487_si_005.cif
_cod_data_source_block           19135_a
_cod_depositor_comments
'Adding full bibliography for 4134704--4134710.cif.'
_cod_database_code               4134704
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              59572
_shelx_hkl_checksum              94140