Binding and Activation of Small Molecules by Three-Coordinate Cr(I)
Wesley H. Monillas; Glenn P. A. Yap; Leonard A. MacAdams; Klaus H. Theopold; Journal of the American Chemical Society 129 (2007) 8090–8091; doi:10.1021/ja0725549

data_4109626
_publ_section_title
;
 Binding and Activation of Small Molecules by Three-Coordinate Cr(I)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8090
_journal_page_last               8091
_journal_paper_doi               10.1021/ja0725549
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C77.5 H107 Cr2 N6 O1.5'
_chemical_formula_weight         1250.69
_chemical_name_common            '[(i-Pr2Ph)2nacnacCr]2(NPh)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.279(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.737(8)
_cell_length_b                   19.148(8)
_cell_length_c                   23.533(8)
_cell_measurement_reflns_used    728
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.19
_cell_measurement_theta_min      2.70
_cell_volume                     7909(6)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.1286
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15046
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.9079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;

 Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
Void space analysis is consistent with 1.5 molecules of 
cocrystallized methyltetrahydrofuran per chromium.
;
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6857
_refine_ls_number_restraints     926
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                3127
_reflns_number_total             6857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0725549si20070525_020758.cif
_cod_data_source_block           klat231s
_cod_original_cell_volume        7909(5)
_cod_original_formula_sum        'C77.50 H107 Cr2 N6 O1.50'
_cod_database_code               4109626