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_4304129
_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         'C48 H84 N6 P4 Si8 Zr2'
_chemical_formula_sum            'C48 H84 N6 P4 Si8 Zr2'
_chemical_formula_weight         1276.25
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      68
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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                   14.290(3)
_cell_length_b                   19.213(2)
_cell_length_c                   24.033(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      77.51
_cell_measurement_theta_min      3.68
_cell_volume                     6598.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'scintilation detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3176
_diffrn_reflns_theta_full        77.51
_diffrn_reflns_theta_max         77.51
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.170
_exptl_absorpt_correction_T_max  0.356
_exptl_absorpt_correction_T_min  0.229
_exptl_absorpt_correction_type   'empirical from intensities'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00009(4)
_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   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2383
_reflns_number_gt                1739
_reflns_number_total             3176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701599t-file001_1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4304129