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_4063536
_publ_section_title
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 Mechanism of the Reaction of Alkynes with a &#x201C;Constrained
 Geometry&#x201D; Zirconaaziridine. PMe3Dissociates More Rapidly from the
 Constrained Geometry Complex than from its Cp2Analogue
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_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            'C17 H30 F3 N O3 S Si Zr'
_chemical_formula_weight         504.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.007(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.168(9)
_cell_length_b                   8.908(4)
_cell_length_c                   25.959(12)
_cell_measurement_temperature    293(2)
_cell_volume                     4618(4)
_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 0.920
_diffrn_measured_fraction_theta_max 0.920
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15252
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.9078
_exptl_absorpt_correction_T_min  0.8476
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.259
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00000(12)
_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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          1.613
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+20.4474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2116
_reflns_number_gt                3445
_reflns_number_total             5279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801009p_si_002.cif
_cod_data_source_block           zrotfs10
_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      C2/c
_cod_database_code               4063536