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_4326749
_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         ' C32 H35 Cl2 N2 P Zr, 2(C3 H3)'
_chemical_formula_sum            'C38 H41 Cl2 N2 P Zr'
_chemical_formula_weight         718.86
_chemical_name_common            Cy5[NPN]DMPZrCl2
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ac'
_symmetry_space_group_name_H-M   'P c m n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.976(4)
_cell_length_b                   14.267(5)
_cell_length_c                   19.098(7)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.890
_cell_measurement_theta_min      2.375
_cell_volume                     3536(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46631
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    .536
_exptl_absorpt_correction_T_max  0.8346
_exptl_absorpt_correction_T_min  0.8142
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0216
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+1.5396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                3953
_reflns_number_total             4392
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201762r_si_002_2.cif
_cod_data_source_block           mf770_0m
_cod_original_formula_sum        ' C38 H41 Cl2 N2 P Zr'
_cod_database_code               4326749