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_4114577
_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_moiety         'C48 H84 N4 P4 Si8 Zr2 '
_chemical_formula_sum            'C48 H84 N4 P4 Si8 Zr2'
_chemical_formula_weight         1248.24
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2001-08-16
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 92.9201(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3696(10)
_cell_length_b                   16.114(2)
_cell_length_c                   19.9855(9)
_cell_measurement_reflns_used    21527
_cell_measurement_temperature    180.2
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.5
_cell_volume                     3013.5(5)
_computing_cell_refinement       'd*TREK (MSC, 1996-1998)'
_computing_data_collection       'd*TREK (MSC, 1996-1998)'
_computing_data_reduction        'd*TREK (MSC, 1996-1998)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      180.2
_diffrn_detector_area_resol_mean 11.76
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.03400
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27604
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  1.001
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
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_refine_diff_density_max         1.23
_refine_diff_density_min         -1.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.685
_refine_ls_goodness_of_fit_ref   2.690
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.050
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      sigma
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_reflns_number_gt                4898
_reflns_number_total             7153
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ja012100q_1.cif
_cod_data_source_block           mf322/Zr2Ph
_cod_original_cell_volume        3013.5(4)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C48 H84 N4 P4 Si8 Zr2 '
_cod_database_code               4114577