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_4326753
_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_sum            'C40 H53 N2 P'
_chemical_formula_weight         592.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.872(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.258(3)
_cell_length_b                   10.699(2)
_cell_length_c                   21.645(6)
_cell_measurement_reflns_used    6079
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      1.3
_cell_volume                     3531.6(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24625
_diffrn_reflns_theta_full        24.84
_diffrn_reflns_theta_max         24.84
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  .985
_exptl_absorpt_correction_T_min  .973
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0323P)^2^+3.5627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                4716
_reflns_number_total             6079
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201762r_si_002_6.cif
_cod_data_source_block           mf834_0m
_cod_original_cell_volume        3531.5(14)
_cod_database_code               4326753