Synthesis, Characterization, and Electronic Structure of Diimine Complexes of Chromium
Kevin A. Kreisel; Glenn P. A. Yap; Klaus H. Theopold; Inorganic Chemistry 47 (2008) 5293–5303; doi:10.1021/ic800302w

data_4305092
_publ_section_title
;
Synthesis, Characterization, and Electronic Structure of Diimine Complexes
of Chromium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5293
_journal_page_last               5303
_journal_paper_doi               10.1021/ic800302w
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C63 H97.5 Cl4 Cr2 N4 O2.75'
_chemical_formula_weight         1200.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.3679(15)
_cell_length_b                   40.969(4)
_cell_length_c                   22.124(2)
_cell_measurement_reflns_used    954
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.83
_cell_measurement_theta_min      2.45
_cell_volume                     13239(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            123794
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.9055
_exptl_absorpt_correction_T_min  0.8230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5132
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_platon_squeeze_details
; 
Data set was treated
with Squeeze filter (Platon) (Spek, A.L. (1990),
Acta Cryst. A46, C-34.)
consistent with initial solutions showing 14 diethyl
ether cocrystallized in the cell.
;
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1239
_refine_ls_number_reflns         23305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0417P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                14736
_reflns_number_total             23305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800302w-file001_1.cif
_cod_data_source_block           klat042s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C63 H97.50 Cl4 Cr2 N4 O2.75'
_cod_database_code               4305092