Mechanism of the Reaction of Alkynes with a "Constrained Geometry" Zirconaaziridine. PMe3Dissociates More Rapidly from the Constrained Geometry Complex than from its Cp2Analogue
Kristian, Kathleen E.; Iimura, Masanori; Cummings, Sarah A.; Norton, Jack R.; Janak, Kevin E.; Pang, Keliang; Organometallics 28 (2009) 493–498; doi:10.1021/om801009p

data_4063539
_publ_section_title
;
 Mechanism of the Reaction of Alkynes with a "Constrained Geometry"
 Zirconaaziridine. PMe3Dissociates More Rapidly from the Constrained
 Geometry Complex than from its Cp2Analogue
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              493
_journal_page_last               498
_journal_paper_doi               10.1021/om801009p
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C42 H48 N2 Si Zr'
_chemical_formula_weight         700.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.656(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5425(18)
_cell_length_b                   14.6123(16)
_cell_length_c                   16.4795(18)
_cell_measurement_temperature    293(2)
_cell_volume                     3651.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0762
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25076
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_correction_T_min  0.9306
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00000(17)
_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   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          1.305
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                5321
_reflns_number_total             8497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801009p_si_005.cif
_cod_data_source_block           minss10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core 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      P2(1)/c
_cod_database_code               4063539