Side-On Bound Dinitrogen Complex of Zirconium Supported by a P2N2 Macrocyclic Ligand
Lara Morello; Maria João Ferreira; Brian O. Patrick; Michael D. Fryzuk; Inorganic Chemistry 47 (2008) 1319–1323; doi:10.1021/ic701599t

data_4304130
_publ_section_title
;
Side-On Bound Dinitrogen Complex of Zirconium Supported by a
P2N2 Macrocyclic Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1319
_journal_page_last               1323
_journal_paper_doi               10.1021/ic701599t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C57 H95 N6 O P4 Si8 Zr2'
_chemical_formula_sum            'C57 H95 N6 O P4 Si8 Zr2'
_chemical_formula_weight         1411.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                88.319(3)
_cell_angle_beta                 75.924(3)
_cell_angle_gamma                72.351(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0869(9)
_cell_length_b                   13.8986(10)
_cell_length_c                   22.8739(15)
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.03
_cell_volume                     3547.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX X8'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31175
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.843
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0024(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+30.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1730
_refine_ls_wR_factor_ref         0.1869
_reflns_number_gt                7019
_reflns_number_total             9167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701599t-file001_2.cif
_cod_data_source_block           compound7
_cod_database_code               4304130