#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:40:09 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180272 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/58/7115837.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7115837
loop_
_publ_author_name
'Irene C. Cai'
'Michael I. Lipschutz'
'T. Don Tilley'
_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            'C42 H76 Cr N2 Si2'
_chemical_formula_weight         717.23
_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                98.9810(10)
_cell_angle_beta                 104.6850(10)
_cell_angle_gamma                118.9100(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6605(3)
_cell_length_b                   10.8266(3)
_cell_length_c                   11.4767(3)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      2.36
_cell_volume                     1059.18(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24671
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.24
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.9687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             394
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+0.4506P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                4302
_reflns_number_total             5882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06615d2.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115837
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.51726(17) -0.02610(17) 0.19492(14) 0.0139(3) Uani 1 1 d .
C2 C 0.63041(18) -0.05626(17) 0.25647(14) 0.0158(3) Uani 1 1 d .
C3 C 0.58548(19) -0.20166(18) 0.24750(15) 0.0198(3) Uani 1 1 d .
H15 H 0.6606 -0.2197 0.2904 0.024 Uiso 1 1 calc R
C4 C 0.4336(2) -0.32251(18) 0.17759(15) 0.0217(4) Uani 1 1 d .
H20 H 0.4066 -0.4216 0.1706 0.026 Uiso 1 1 calc R
C5 C 0.32365(19) -0.29675(18) 0.11914(15) 0.0201(3) Uani 1 1 d .
H7 H 0.2201 -0.3793 0.0720 0.024 Uiso 1 1 calc R
C6 C 0.35987(18) -0.15139(17) 0.12692(14) 0.0163(3) Uani 1 1 d .
C7 C 0.22496(18) -0.13097(19) 0.08567(15) 0.0199(3) Uani 1 1 d .
H10 H 0.2688 -0.0242 0.0910 0.024 Uiso 1 1 calc R
C8 C 0.1428(2) -0.1618(2) 0.17943(19) 0.0315(4) Uani 1 1 d .
H23A H 0.0602 -0.1428 0.1567 0.047 Uiso 1 1 calc R
H23B H 0.2176 -0.0961 0.2661 0.047 Uiso 1 1 calc R
H23C H 0.0979 -0.2663 0.1755 0.047 Uiso 1 1 calc R
C9 C 0.1082(2) -0.2286(2) -0.05015(18) 0.0315(4) Uani 1 1 d .
H17A H 0.1613 -0.2079 -0.1098 0.047 Uiso 1 1 calc R
H17B H 0.0279 -0.2064 -0.0711 0.047 Uiso 1 1 calc R
H17C H 0.0603 -0.3341 -0.0569 0.047 Uiso 1 1 calc R
C10 C 0.79831(18) 0.06847(18) 0.33477(15) 0.0192(3) Uani 1 1 d .
H13 H 0.8128 0.1639 0.3243 0.023 Uiso 1 1 calc R
C11 C 0.9112(2) 0.0439(2) 0.28998(18) 0.0291(4) Uani 1 1 d .
H21A H 0.9056 -0.0445 0.3062 0.044 Uiso 1 1 calc R
H21B H 1.0170 0.1316 0.3368 0.044 Uiso 1 1 calc R
H21C H 0.8830 0.0289 0.1984 0.044 Uiso 1 1 calc R
C12 C 0.8390(2) 0.0862(2) 0.47695(16) 0.0261(4) Uani 1 1 d .
H9A H 0.7677 0.1025 0.5058 0.039 Uiso 1 1 calc R
H9B H 0.9455 0.1719 0.5258 0.039 Uiso 1 1 calc R
H9C H 0.8300 -0.0046 0.4901 0.039 Uiso 1 1 calc R
C13 C 0.65853(18) 0.31153(17) 0.44193(14) 0.0171(3) Uani 1 1 d .
H12 H 0.7588 0.3176 0.4689 0.020 Uiso 1 1 calc R
C14 C 0.5469(2) 0.18237(19) 0.47785(16) 0.0230(4) Uani 1 1 d .
H14A H 0.5944 0.1985 0.5685 0.034 Uiso 1 1 calc R
H14B H 0.5251 0.0879 0.4265 0.034 Uiso 1 1 calc R
H14C H 0.4500 0.1784 0.4615 0.034 Uiso 1 1 calc R
C15 C 0.6927(2) 0.46085(19) 0.52121(16) 0.0250(4) Uani 1 1 d .
H8A H 0.5980 0.4613 0.4971 0.037 Uiso 1 1 calc R
H8B H 0.7728 0.5435 0.5048 0.037 Uiso 1 1 calc R
H8C H 0.7292 0.4726 0.6121 0.037 Uiso 1 1 calc R
C16 C 0.75972(18) 0.43186(17) 0.23076(15) 0.0178(3) Uani 1 1 d .
H19 H 0.7457 0.3864 0.1419 0.021 Uiso 1 1 calc R
C17 C 0.92146(18) 0.47657(19) 0.31746(16) 0.0224(4) Uani 1 1 d .
H11A H 0.9992 0.5420 0.2875 0.034 Uiso 1 1 calc R
H11B H 0.9234 0.3866 0.3149 0.034 Uiso 1 1 calc R
H11C H 0.9447 0.5295 0.4052 0.034 Uiso 1 1 calc R
C18 C 0.7607(2) 0.57490(19) 0.23349(18) 0.0252(4) Uani 1 1 d .
H18A H 0.7685 0.6212 0.3177 0.038 Uiso 1 1 calc R
H18B H 0.6646 0.5496 0.1683 0.038 Uiso 1 1 calc R
H18C H 0.8496 0.6450 0.2162 0.038 Uiso 1 1 calc R
C19 C 0.43153(18) 0.31123(19) 0.20852(15) 0.0193(3) Uani 1 1 d .
H24 H 0.4810 0.4214 0.2446 0.023 Uiso 1 1 calc R
C20 C 0.2965(2) 0.2404(2) 0.25319(17) 0.0259(4) Uani 1 1 d .
H22A H 0.2260 0.2723 0.2228 0.039 Uiso 1 1 calc R
H22B H 0.3368 0.2724 0.3466 0.039 Uiso 1 1 calc R
H22C H 0.2403 0.1313 0.2187 0.039 Uiso 1 1 calc R
C21 C 0.3691(2) 0.2748(2) 0.06273(15) 0.0238(4) Uani 1 1 d .
H16A H 0.3123 0.1666 0.0209 0.036 Uiso 1 1 calc R
H16B H 0.4559 0.3255 0.0358 0.036 Uiso 1 1 calc R
H16C H 0.2994 0.3090 0.0388 0.036 Uiso 1 1 calc R
N1 N 0.55810(14) 0.11313(14) 0.18089(12) 0.0144(3) Uani 1 1 d .
Si1 Si 0.59603(5) 0.28118(5) 0.26438(4) 0.01342(10) Uani 1 1 d .
Cr1 Cr 0.5000 0.0000 0.0000 0.01427(10) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C6 118.89(13) . .
N1 C1 C2 122.76(13) . .
C6 C1 C2 117.47(14) . .
N1 C1 Cr1 60.78(7) . .
C6 C1 Cr1 83.80(9) . .
C2 C1 Cr1 117.57(10) . .
C3 C2 C1 119.79(14) . .
C3 C2 C10 118.52(14) . .
C1 C2 C10 121.67(14) . .
C2 C3 C4 122.11(15) . .
C2 C3 H15 118.9 . .
C4 C3 H15 118.9 . .
C5 C4 C3 119.22(15) . .
C5 C4 H20 120.4 . .
C3 C4 H20 120.4 . .
C4 C5 C6 121.87(15) . .
C4 C5 H7 119.1 . .
C6 C5 H7 119.1 . .
C5 C6 C1 119.48(14) . .
C5 C6 C7 117.53(14) . .
C1 C6 C7 121.83(14) . .
C9 C7 C6 114.09(14) . .
C9 C7 C8 109.83(15) . .
C6 C7 C8 109.05(14) . .
C9 C7 H10 107.9 . .
C6 C7 H10 107.9 . .
C8 C7 H10 107.9 . .
C7 C8 H23A 109.5 . .
C7 C8 H23B 109.5 . .
H23A C8 H23B 109.5 . .
C7 C8 H23C 109.5 . .
H23A C8 H23C 109.5 . .
H23B C8 H23C 109.5 . .
C7 C9 H17A 109.5 . .
C7 C9 H17B 109.5 . .
H17A C9 H17B 109.5 . .
C7 C9 H17C 109.5 . .
H17A C9 H17C 109.5 . .
H17B C9 H17C 109.5 . .
C2 C10 C12 111.23(13) . .
C2 C10 C11 112.21(13) . .
C12 C10 C11 109.34(14) . .
C2 C10 H13 108.0 . .
C12 C10 H13 108.0 . .
C11 C10 H13 108.0 . .
C10 C11 H21A 109.5 . .
C10 C11 H21B 109.5 . .
H21A C11 H21B 109.5 . .
C10 C11 H21C 109.5 . .
H21A C11 H21C 109.5 . .
H21B C11 H21C 109.5 . .
C10 C12 H9A 109.5 . .
C10 C12 H9B 109.5 . .
H9A C12 H9B 109.5 . .
C10 C12 H9C 109.5 . .
H9A C12 H9C 109.5 . .
H9B C12 H9C 109.5 . .
C14 C13 C15 110.04(13) . .
C14 C13 Si1 114.23(11) . .
C15 C13 Si1 113.10(11) . .
C14 C13 H12 106.3 . .
C15 C13 H12 106.3 . .
Si1 C13 H12 106.3 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H8A 109.5 . .
C13 C15 H8B 109.5 . .
H8A C15 H8B 109.5 . .
C13 C15 H8C 109.5 . .
H8A C15 H8C 109.5 . .
H8B C15 H8C 109.5 . .
C18 C16 C17 108.55(13) . .
C18 C16 Si1 116.07(11) . .
C17 C16 Si1 113.06(11) . .
C18 C16 H19 106.1 . .
C17 C16 H19 106.1 . .
Si1 C16 H19 106.1 . .
C16 C17 H11A 109.5 . .
C16 C17 H11B 109.5 . .
H11A C17 H11B 109.5 . .
C16 C17 H11C 109.5 . .
H11A C17 H11C 109.5 . .
H11B C17 H11C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C21 110.08(13) . .
C20 C19 Si1 118.91(12) . .
C21 C19 Si1 111.44(11) . .
C20 C19 H24 105.0 . .
C21 C19 H24 105.0 . .
Si1 C19 H24 105.0 . .
C19 C20 H22A 109.5 . .
C19 C20 H22B 109.5 . .
H22A C20 H22B 109.5 . .
C19 C20 H22C 109.5 . .
H22A C20 H22C 109.5 . .
H22B C20 H22C 109.5 . .
C19 C21 H16A 109.5 . .
C19 C21 H16B 109.5 . .
H16A C21 H16B 109.5 . .
C19 C21 H16C 109.5 . .
H16A C21 H16C 109.5 . .
H16B C21 H16C 109.5 . .
C1 N1 Si1 139.14(10) . .
C1 N1 Cr1 81.59(8) . .
Si1 N1 Cr1 137.87(8) . .
N1 Si1 C13 111.11(7) . .
N1 Si1 C19 114.81(7) . .
C13 Si1 C19 110.23(7) . .
N1 Si1 C16 106.54(7) . .
C13 Si1 C16 109.80(7) . .
C19 Si1 C16 103.97(7) . .
N1 Cr1 N1 180.00(8) 2_655 .
N1 Cr1 C1 142.37(5) 2_655 .
N1 Cr1 C1 37.63(5) . .
N1 Cr1 C1 37.63(5) 2_655 2_655
N1 Cr1 C1 142.37(5) . 2_655
C1 Cr1 C1 180.00(16) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.402(2) .
C1 C6 1.439(2) .
C1 C2 1.443(2) .
C1 Cr1 2.2709(14) .
C2 C3 1.383(2) .
C2 C10 1.518(2) .
C3 C4 1.394(2) .
C3 H15 0.9500 .
C4 C5 1.370(2) .
C4 H20 0.9500 .
C5 C6 1.409(2) .
C5 H7 0.9500 .
C6 C7 1.528(2) .
C7 C9 1.525(2) .
C7 C8 1.531(2) .
C7 H10 1.0000 .
C8 H23A 0.9800 .
C8 H23B 0.9800 .
C8 H23C 0.9800 .
C9 H17A 0.9800 .
C9 H17B 0.9800 .
C9 H17C 0.9800 .
C10 C12 1.533(2) .
C10 C11 1.538(2) .
C10 H13 1.0000 .
C11 H21A 0.9800 .
C11 H21B 0.9800 .
C11 H21C 0.9800 .
C12 H9A 0.9800 .
C12 H9B 0.9800 .
C12 H9C 0.9800 .
C13 C14 1.537(2) .
C13 C15 1.542(2) .
C13 Si1 1.8960(16) .
C13 H12 1.0000 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H8A 0.9800 .
C15 H8B 0.9800 .
C15 H8C 0.9800 .
C16 C18 1.539(2) .
C16 C17 1.540(2) .
C16 Si1 1.9081(16) .
C16 H19 1.0000 .
C17 H11A 0.9800 .
C17 H11B 0.9800 .
C17 H11C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 C20 1.534(2) .
C19 C21 1.541(2) .
C19 Si1 1.9075(16) .
C19 H24 1.0000 .
C20 H22A 0.9800 .
C20 H22B 0.9800 .
C20 H22C 0.9800 .
C21 H16A 0.9800 .
C21 H16B 0.9800 .
C21 H16C 0.9800 .
N1 Si1 1.7146(13) .
N1 Cr1 2.0036(12) .
Cr1 N1 2.0036(12) 2_655
Cr1 C1 2.2709(14) 2_655
