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_7115839
_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            'C58 H116 Cr K N2 O8 Si2'
_chemical_formula_weight         1116.81
_chemical_properties_physical    Air-sensitive
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8187(7)
_cell_length_b                   17.0756(8)
_cell_length_c                   25.0015(13)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.39
_cell_volume                     6753.3(6)
_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 0.836
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54941
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.70
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9969
_exptl_absorpt_correction_T_min  0.9664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2452
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethoxyethane/pentane'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         16443
_refine_ls_number_restraints     158
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+7.7090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.1995
_reflns_number_gt                12960
_reflns_number_total             16443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06615d2.cif
_cod_data_source_block           shelxl_b
_cod_original_cell_volume        6753.2(6)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7115839