Enforced η1-Fluorenyl and Indenyl Coordination to Zirconium: Geometrically Constrained and Sterically Expanded Complexes Derived from the Bifunctional (FluPPh2NAr)−and (IndPPh2NAr)−Ligands
Oulié, Pascal; Freund, Christelle; Saffon, Nathalie; Martin-Vaca, Blanca; Maron, Laurent; Bourissou, Didier; Organometallics 26 (2007) 6793–; doi:10.1021/om700974g

data_4074088
_publ_section_title
;
 Enforced \h1-Fluorenyl and Indenyl Coordination to Zirconium:
 Geometrically Constrained and Sterically Expanded Complexes Derived from
 the Bifunctional (FluPPh2NAr)&#x2212;and (IndPPh2NAr)&#x2212;Ligands
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6793
_journal_paper_doi               10.1021/om700974g
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C52 H44 N P Zr'
_chemical_formula_weight         805.07
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.602(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9869(14)
_cell_length_b                   18.293(3)
_cell_length_c                   22.616(3)
_cell_measurement_reflns_used    868
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.467
_cell_measurement_theta_min      2.227
_cell_volume                     4047.3(10)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker CCD 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  0.2280
_diffrn_reflns_av_sigmaI/netI    0.2428
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15744
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.602190
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1871
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                2268
_reflns_number_total             4873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700974g-file006.cif
_cod_data_source_block           5a
_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 2.4.1 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      P2(1)/c
_cod_database_code               4074088