A bis(amido) ligand set that supports two-coordinate chromium in the +1, +2, and +3 oxidation states
Irene C. Cai; Michael I. Lipschutz; T. Don Tilley; Chem.Commun. 50 (2014) 13062–; doi:10.1039/C4cc06615D

data_7115838
_publ_section_title
;
 A bis(amido) ligand set that supports two-coordinate chromium in the +1,
 +2, and +3 oxidation states
;
_journal_name_full               Chem.Commun.
_journal_page_first              13062
_journal_paper_doi               10.1039/C4cc06615D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C69 H77 B Cr F21 N2 Si2'
_chemical_formula_weight         1452.32
_chemical_properties_physical    Air-sensitive
_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                67.150(3)
_cell_angle_beta                 89.637(3)
_cell_angle_gamma                69.398(3)
_cell_formula_units_Z            2
_cell_length_a                   13.4838(8)
_cell_length_b                   15.8748(9)
_cell_length_c                   18.4544(10)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.26
_cell_volume                     3368.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55268
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1502
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-difluorobenzene/hexamethyldisiloxane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.339
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         12395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.079
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+6.1162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                10373
_reflns_number_total             12395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06615d2.cif
_cod_data_source_block           shelxl_a
_cod_original_cell_volume        3368.3(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115838