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_7053810
_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         'C39 H35 Cl2 Cr N2 O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C47 H51 Cl2 Cr N2 O4 P2'
_chemical_formula_weight         892.74
_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                72.651(1)
_cell_angle_beta                 83.444(1)
_cell_angle_gamma                80.124(1)
_cell_formula_units_Z            2
_cell_length_a                   9.412(1)
_cell_length_b                   13.128(1)
_cell_length_c                   18.731(1)
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2171.5(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16829
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.8968
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+6.3290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2261
_reflns_number_gt                5263
_reflns_number_total             7856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904619dsup1.cif
_cod_data_source_block           ckl-122
_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               7053810