2-Indenylidene Pincer Complexes of Zirconium and Palladium
Pascal Oulié; Noel Nebra; Nathalie Saffon; Laurent Maron; Blanca Martin-Vaca; Didier Bourissou; Journal of the American Chemical Society 131 (2009) 3493–3498; doi:10.1021/ja809892a

data_4104028
_publ_section_title
;
 2-Indenylidene Pincer Complexes of Zirconium and Palladium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3493
_journal_page_last               3498
_journal_paper_doi               10.1021/ja809892a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C47 H51 N O0.5 P2 Pd S2'
_chemical_formula_weight         870.35
_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                 90.580(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3074(4)
_cell_length_b                   14.8453(5)
_cell_length_c                   25.2573(7)
_cell_measurement_reflns_used    2220
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.65
_cell_measurement_theta_min      2.26
_cell_volume                     4239.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1960
_diffrn_reflns_av_sigmaI/netI    0.1436
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42235
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         7158
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                3548
_reflns_number_total             7158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809892a_si_004.cif
_cod_data_source_block           noel3m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C47 H51 N O0.50 P2 Pd S2'
_cod_database_code               4104028