Phosphorus Phenyl-Group Activation by Reduced Zirconium and Niobium Complexes Stabilized by the [P2N2] Macrocycle
Michael D. Fryzuk; Christopher M. Kozak; Parisa Mehrkhodavandi; Lara Morello; Brian O. Patrick; Steven J. Rettig; Journal of the American Chemical Society 124 (2002) 516–517; doi:10.1021/ja012100q

data_4114578
_publ_section_title
;
 Phosphorus Phenyl-Group Activation by Reduced Zirconium and Niobium
 Complexes Stabilized by the [P2N2] Macrocycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              516
_journal_page_last               517
_journal_paper_doi               10.1021/ja012100q
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C48 H84 N4 Nb2 P4 Si8'
_chemical_formula_weight         1251.61
_chemical_name_systematic
; 
 ? 
;
_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                86.865(2)
_cell_angle_beta                 88.448(3)
_cell_angle_gamma                86.208(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1860(6)
_cell_length_b                   11.2073(6)
_cell_length_c                   13.2219(7)
_cell_measurement_reflns_used    7361
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.6
_cell_volume                     1503.40(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.805
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5843
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7735
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       platelet
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5843
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.6260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                5097
_reflns_number_total             5843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012100q_2.cif
_cod_data_source_block           mf462/Nb2Ph
_cod_database_code               4114578