Chromium (iii)-bis(iminophosphoranyl)methanido complexes: synthesis, X-ray crystal structures and catalytic ethylene oligomerization
Klemps, Christian; Buchard, Antoine; Houdard, Romaric; Auffrant, Audrey; Mézailles, Nicolas; Le Goff, Xavier Frédéric; Ricard, Louis; Saussine, Lucien; Magna, Lionel; Le Floch, Pascal; New Journal of Chemistry 33 (2009) 1748–; doi:10.1039/b904619d

data_7053808
_publ_section_title
;
 Chromium (iii)-bis(iminophosphoranyl)methanido complexes: synthesis,
 X-ray crystal structures and catalytic ethylene oligomerization
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1748
_journal_paper_doi               10.1039/b904619d
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         C62H70Cl4Cr2N4P4,6(CH2Cl2)?
_chemical_formula_sum            'C68 H82 Cl16 Cr2 N4 P4'
_chemical_formula_weight         1750.46
_chemical_name_systematic
;
?
;
_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                77.252(1)
_cell_angle_beta                 69.776(1)
_cell_angle_gamma                69.642(1)
_cell_formula_units_Z            1
_cell_length_a                   12.779(1)
_cell_length_b                   12.956(1)
_cell_length_c                   13.700(1)
_cell_measurement_reflns_used    8389
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1982.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29661
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.9122
_exptl_absorpt_correction_T_min  0.8205
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0006(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         11583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0491P)^2^+0.7747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                9507
_reflns_number_total             11583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904619dsup1.cif
_cod_data_source_block           nm2546
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7053808