Insertion of Acetonitrile into the Zr−P Bond of [Cp°2ZrCl(PHCy)] (Cy = Cyclohexyl, Cp° = η5-C5EtMe4) Followed by PHCy Elimination To Give [Cp°2(Cl)Zr(μ-NCMe−CMeN)Zr(Cl)Cp°2]†
Segerer, Ulrike; Blaurock, Steffen; Sieler, Joachim; Hey-Hawkins, Evamarie; Organometallics 18 (1999) 2838–; doi:10.1021/om9901271

data_4077773
_publ_section_title
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 Insertion of Acetonitrile into the Zr&#x2212;P Bond of [Cp\%2ZrCl(PHCy)]
 (Cy = Cyclohexyl, Cp\% = \h5-C5EtMe4) Followed by PHCy Elimination To
 Give [Cp\%2(Cl)Zr(\m-NCMe&#x2212;CMeN)Zr(Cl)Cp\%2]&#x2020;
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_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              2838
_journal_paper_doi               10.1021/om9901271
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C24 H37 Cl N Zr'
_chemical_formula_weight         466.22
_chemical_name_systematic
; 
 ? 
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_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 C17,C18,C19,C20,C21,C22'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.6080(10)
_cell_angle_beta                 77.9410(10)
_cell_angle_gamma                72.72
_cell_formula_units_Z            2
_cell_length_a                   8.7492(8)
_cell_length_b                   10.6231(11)
_cell_length_c                   13.6351(10)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     1150.03(18)
_computing_cell_refinement       'SAINT (AXS-BRUKER)'
_computing_data_collection       'SMART (AXS-BRUKER)'
_computing_data_reduction        'SAINT (AXS-BRUKER)'
_computing_molecular_graphics    'XP (AXS-BRUKER)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.827
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_device_type  'CCD-Diffractometer (AXS-BRUKER)'
_diffrn_measurement_method       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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5174
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.8639
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0003(7)
_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   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.171
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+4.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                3432
_reflns_number_total             3793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9901271.cif
_cod_data_source_block           cd133
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+4.3081P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+4.3081P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1150.02(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077773