Nucleophilic Reactivity of the Multiply Bonded Carbon Center in Group 4−Pincer Bis(iminophosphorano)methanediide Complexes
Kamalesh Babu, Ruppa P.; McDonald, Robert; Cavell, Ronald G.; Organometallics 19 (2000) 3462–; doi:10.1021/om000181d

data_4077504
_publ_section_title
;
 Nucleophilic Reactivity of the Multiply Bonded Carbon Center in Group
 4&#x2212;Pincer Bis(iminophosphorano)methanediide Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3462
_journal_paper_doi               10.1021/om000181d
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C58.5 H80 Cl2 N4 O P2 Si2 Zr'
_chemical_formula_weight         1135.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.0569(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5636(8)
_cell_length_b                   18.4194(12)
_cell_length_c                   28.0498(19)
_cell_measurement_reflns_used    8079
_cell_measurement_temperature    193(2)
_cell_volume                     5959.5(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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            46944
_diffrn_reflns_theta_full        25.72
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9622
_exptl_absorpt_correction_T_min  0.7310
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2396
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         11320
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.134
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1657
_reflns_number_gt                7421
_reflns_number_total             11320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000181d.cif
_cod_data_source_block           rgc9902
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C58.50 H80 Cl2 N4 O P2 Si2 Zr'
_cod_database_code               4077504