Heterometallic Aluminum‒Chromium Phenazine and Thiophenazine Complexes. Formation of a Tetranuclear Chromium(I) Sandwich Complex
Shuster, Vladimir; Gambarotta, Sandro; Nikiforov, Grigory B.; Budzelaar, Peter H. M.; Organometallics 32 (2013) 2329–; doi:10.1021/om3012097

data_4080407
_publ_section_title
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 Heterometallic Aluminum--Chromium Phenazine and Thiophenazine Complexes.
 Formation of a Tetranuclear Chromium(I) Sandwich Complex
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_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2329
_journal_paper_doi               10.1021/om3012097
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C32 H36 Al2 Cl2 Cr N2 S2'
_chemical_formula_weight         689.61
_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                106.479(2)
_cell_angle_beta                 95.036(2)
_cell_angle_gamma                107.048(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3503(13)
_cell_length_b                   9.9256(14)
_cell_length_c                   10.0618(14)
_cell_measurement_reflns_used    6660
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.79
_cell_measurement_theta_min      2.15
_cell_volume                     841.1(2)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7840
_diffrn_reflns_theta_full        24.79
_diffrn_reflns_theta_max         24.79
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.9023
_exptl_absorpt_correction_T_min  0.8727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            blue_purple
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+0.6534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                2492
_reflns_number_total             2807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3012097_si_001.cif
_cod_data_source_block           sg3914
_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 

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      P-1
_cod_database_code               4080407