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_4074087
_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            'C33 H34 N P'
_chemical_formula_weight         475.58
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.706(3)
_cell_angle_beta                 82.801(3)
_cell_angle_gamma                81.750(2)
_cell_formula_units_Z            4
_cell_length_a                   9.0146(11)
_cell_length_b                   17.367(2)
_cell_length_c                   18.711(2)
_cell_measurement_reflns_used    1604
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.116
_cell_measurement_theta_min      2.290
_cell_volume                     2692.6(5)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0850
_diffrn_reflns_av_sigmaI/netI    0.1816
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11111
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         5.12
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         6891
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                3302
_reflns_number_total             6891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700974g-file005.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        2692.5(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074087