Crystal structure of an isomeric bis[(η 5:η 1-6,6-di-p-tolylpentafulvene)(η 5-pentamethylcyclopentadienyl)titanium(III)]-μ 2,η 1:η 1-dinitrogen complex, C60H66N2Ti2
Oswald, Tim; Frey, Annika; Schmidtmann, Marc; Beckhaus, Rüdiger; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 1095–1097; doi:10.1515/ncrs-2016-0074

data_8107112
_publ_section_title
;
 Crystal structure of an isomeric bis[(\h 5:\h
 1-6,6-di-p-tolylpentafulvene)(\h
 5-pentamethylcyclopentadienyl)titanium(III)]-\m 2,\h 1:\h 1-dinitrogen
 complex, C60H66N2Ti2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1095
_journal_page_last               1097
_journal_paper_doi               10.1515/ncrs-2016-0074
_journal_volume                  231
_journal_year                    2016
_chemical_formula_structural     Ti2N2(C10H15)2(C20H18)2
_chemical_formula_sum            'C60 H66 N2 Ti2'
_chemical_formula_weight         910.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                66.7623(13)
_cell_angle_beta                 89.0505(13)
_cell_angle_gamma                80.9952(13)
_cell_formula_units_Z            1
_cell_length_a                   8.8070(3)
_cell_length_b                   11.9544(5)
_cell_length_c                   12.3447(5)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.17
_cell_measurement_theta_min      2.75
_cell_volume                     1178.06(8)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48555
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.029
_diffrn_reflns_theta_min         1.798
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         8199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0600P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6433
_reflns_number_total             8199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0074_suppl.cif
_cod_data_source_block           to88
_cod_database_code               8107112
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              48257
_shelx_hkl_checksum              88900