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_4326750
_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         36CH94N8P2Zr2
_chemical_formula_sum            'C36 H47 N4 P Zr'
_chemical_formula_weight         657.97
_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                89.473(2)
_cell_angle_beta                 88.110(2)
_cell_angle_gamma                72.927(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5299(4)
_cell_length_b                   11.7212(4)
_cell_length_c                   12.9070(5)
_cell_measurement_reflns_used    7521
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.8
_cell_volume                     1666.53(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43830
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.8408
_exptl_absorpt_correction_T_min  0.7918
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       prisim
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.8522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                7521
_reflns_number_total             7969
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201762r_si_002_3.cif
_cod_data_source_block           mf776_0m
_cod_original_cell_volume        1666.53(10)
_cod_database_code               4326750