One- and two-step [2 + 2] cycloaddition reactions of group 4 imides with the phosphaalkyne ButCP. Crystal and molecular structures of [Zr(η5-C5H5)2(PCButNC6H3Me2-2,6)] and [TiCl2(P2C2But2NBut)(py)] (py) = pyridine)
Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Nixon, John F.; James Wilson, D.; Mountford, Philip; Chemical Communications  (1999) 661–; doi:10.1039/a900648f

data_7110467
_publ_section_title
;
 One- and two-step [2 + 2] cycloaddition reactions of group 4 imides with
 the phosphaalkyne ButCP. Crystal and molecular structures of
 [Zr(\h5-C5H5)2(PCButNC6H3Me2-2,6)] and [TiCl2(P2C2But2NBut)(py)] (py) =
 pyridine)
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              661
_journal_paper_doi               10.1039/a900648f
_journal_year                    1999
_chemical_formula_structural     '[Zr(C5H5)2(C6H3Me2NP=CtBu)]'
_chemical_formula_sum            'C23 H28 N P Zr'
_chemical_formula_weight         440.65
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.01(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.622(3)
_cell_length_b                   21.830(8)
_cell_length_c                   8.389(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     2035.3(14)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3811
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.647
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.834
_refine_ls_goodness_of_fit_obs   0.817
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_restrained_S_obs      0.817
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+8.2446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1375
_refine_ls_wR_factor_obs         0.1141
_reflns_number_observed          2651
_reflns_number_total             3563
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900648fsup1.cif
_cod_data_source_block           fgnc/jfn-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+8.2446P] 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^)+(0.0782P)^2^+8.2446P] 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        2035.3(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110467