Insertion Reactions and Catalytic Hydrophosphination by Triamidoamine-Supported Zirconium Complexes
Roering, Andrew J.; Leshinski, Sarah E.; Chan, Stephanie M.; Shalumova, Tamila; MacMillan, Samantha N.; Tanski, Joseph M.; Waterman, Rory; Organometallics 29 (2010) 2557–; doi:10.1021/om100216f

data_4065961
_publ_section_title
;
 Insertion Reactions and Catalytic Hydrophosphination by
 Triamidoamine-Supported Zirconium Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2557
_journal_paper_doi               10.1021/om100216f
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C34 H54 N5 P Si3 Zr'
_chemical_formula_weight         739.28
_chemical_name_common            '(N3N)ZrN=C(PPh2)Ph, 5'
_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                88.3820(10)
_cell_angle_beta                 87.4270(10)
_cell_angle_gamma                69.1720(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1235(4)
_cell_length_b                   12.0108(5)
_cell_length_c                   17.5314(8)
_cell_measurement_reflns_used    9475
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.27
_cell_volume                     1990.19(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26287
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.8989
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.7385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                8657
_reflns_number_total             9812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100216f_si_001.cif
_cod_data_source_block           rw553zr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065961