Redox non-innocence permits catalytic nitrene carbonylation by (dadi)TiNAd (Ad = adamantyl)
Heins, Spencer P.; Wolczanski, Peter T.; Cundari, Thomas R.; MacMillan, Samantha N.; Chem. Sci. 8 (2017) 3410–; doi:10.1039/C6SC05610E

data_1545511
_publ_section_title
;
 Redox non-innocence permits catalytic nitrene carbonylation by
 (dadi)Ti&#xE001;NAd (Ad = adamantyl)
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3410
_journal_paper_doi               10.1039/C6SC05610E
_journal_volume                  8
_journal_year                    2017
_chemical_formula_sum            'C47 H62 N6 Ti'
_chemical_formula_weight         758.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                100.164(3)
_cell_angle_beta                 104.521(2)
_cell_angle_gamma                95.151(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2323(6)
_cell_length_b                   13.2844(7)
_cell_length_c                   16.9919(9)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.53
_cell_volume                     2179.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29680
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.804
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       Block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.300
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_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.375
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_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8887
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6756
_reflns_number_total             8887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc05610e2.cif
_cod_data_source_block           sh30_a
_cod_depositor_comments
'Adding full bibliography for 1545511--1545513.cif.'
_cod_database_code               1545511
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              33211