Isolation and Characterization of a Class II Mixed-Valence Chromium(I)/(II) Self-Activating Ethylene Trimerization Catalyst
Thapa, Indira; Gambarotta, Sandro; Korobkov, Ilia; Murugesu, Muralee; Budzelaar, Peter; Organometallics 31 (2012) 486–; doi:10.1021/om201181n

data_4068182
_publ_section_title
;
 Isolation and Characterization of a Class II Mixed-Valence
 Chromium(I)/(II) Self-Activating Ethylene Trimerization Catalyst
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              486
_journal_paper_doi               10.1021/om201181n
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C51 H66 Cr2 N3 P4'
_chemical_formula_weight         948.95
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.7483(6)
_cell_length_b                   21.7483(6)
_cell_length_c                   21.7483(6)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.65
_cell_volume                     10286.7(5)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0587
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_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            160751
_diffrn_reflns_theta_full        33.15
_diffrn_reflns_theta_max         33.15
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.267
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     181
_refine_ls_number_reflns         6497
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_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+5.3810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                4814
_reflns_number_total             6497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201181n_si_002.cif
_cod_data_source_block           sg113
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' 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_sg_symbol_H-M      Pa-3
_cod_database_code               4068182