Synthesis and reactivity of titanium- and zirconium-dinitrogen complexes bearing anionic pyrrole-based PNP-type pincer ligands.
Sekiguchi, Yoshiya; Meng, Fanqiang; Tanaka, Hiromasa; Eizawa, Aya; Arashiba, Kazuya; Nakajima, Kazunari; Yoshizawa, Kazunari; Nishibayashi, Yoshiaki; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11322–11326; doi:10.1039/c8dt02739k

data_7047122
_publ_section_title
;
 Synthesis and reactivity of titanium- and zirconium-dinitrogen complexes
 bearing anionic pyrrole-based PNP-type pincer ligands.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11322
_journal_page_last               11326
_journal_paper_doi               10.1039/c8dt02739k
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C54 H94 N4 P4 Ti2'
_chemical_formula_sum            'C54 H94 N4 P4 Ti2'
_chemical_formula_weight         1019.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-06-06 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.9662(3)
_cell_length_b                   22.1194(4)
_cell_length_c                   22.1259(4)
_cell_measurement_reflns_used    53470
_cell_measurement_temperature    183
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      1.82
_cell_volume                     6345.8(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      183
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.458
_diffrn_reflns_theta_min         2.058
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2200.00
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_details
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     602
_refine_ls_number_reflns         14499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12772
_reflns_number_total             14499
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c8dt02739k2.cif
_cod_data_source_block           20171203Ti2PNP2Cp2N2
_cod_depositor_comments
'Adding full bibliography for 7047117--7047122.cif.'
_cod_database_code               7047122
_shelx_res_checksum              16949
_shelx_fab_checksum              55153