New Cyclopentenyl-Linked [NPN] Ligands and Their Coordination Chemistry with Zirconium: Synthesis of a Dinuclear Side-On-Bound Dinitrogen Complex
Ting Zhu; Truman C. Wambach; Michael D. Fryzuk; Inorganic Chemistry 50 (2011) 11212–11221; doi:10.1021/ic201762r

data_4326751
_publ_contact_author_email       fryzuk@chem.ubc.ca
_publ_contact_author_name        'Michael D. Fryzuk'
_publ_section_title
;
 New Cyclopentenyl-Linked [NPN] Ligands and Their Coordination Chemistry
 with Zirconium: Synthesis of a Dinuclear Side-On-Bound Dinitrogen Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11212
_journal_page_last               11221
_journal_paper_doi               10.1021/ic201762r
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C44 H63 N4 P Zr'
_chemical_formula_sum            'C44 H63 N4 P Zr'
_chemical_formula_weight         770.17
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.108(2)
_cell_angle_beta                 99.135(2)
_cell_angle_gamma                90.293(2)
_cell_formula_units_Z            4
_cell_length_a                   10.9989(4)
_cell_length_b                   17.8519(6)
_cell_length_c                   21.4760(9)
_cell_measurement_reflns_used    14397
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     4108.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker x8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52990
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.9046
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                9998
_reflns_number_total             14397
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201762r_si_002_4.cif
_cod_data_source_block           mf795_0m
_cod_original_sg_symbol_Hall     -P1
_cod_original_formula_sum        ' C44 H63 N4 P Zr'
_cod_database_code               4326751