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#$Date: 2016-03-21 08:04:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178593 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/04/4070403.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_4070403
loop_
_publ_author_name
'MacLeod, K. Cory'
'Conway, Julia L.'
'Tang, Liming'
'Smith, Joshua J.'
'Corcoran, Liam D.'
'Ballem, Katherine H. D.'
'Patrick, Brian O.'
'Smith, Kevin M.'
_publ_section_title
;
 Reactivity Consequences of Steric Reduction in Cyclopentadienyl Chromium
 β-Diketiminate Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6798
_journal_paper_doi               10.1021/om900788c
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C28 H34 Cr I N2'
_chemical_formula_weight         577.47
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   14.7580(10)
_cell_length_b                   21.794(2)
_cell_length_c                   7.9989(7)
_cell_measurement_reflns_used    15215
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.70
_cell_volume                     2572.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.0126
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5004
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0226
_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)+(0.0334P)²+1.8380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                2618
_reflns_number_total             2924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900788c_si_001.cif
_cod_data_source_block           2c
_cod_original_sg_symbol_H-M      'P nma'
_cod_database_code               4070403
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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 0.15279(13) 0.62368(8) 0.6824(2) 0.0115(3) Uani 1 1 d .
C2 C 0.18994(14) 0.57569(9) 0.5884(3) 0.0167(4) Uani 1 1 d .
C3 C 0.14856(14) 0.51787(9) 0.5956(3) 0.0193(4) Uani 1 1 d .
H3 H 0.1738 0.4852 0.5323 0.023 Uiso 1 1 calc R
C4 C 0.07216(14) 0.50657(8) 0.6918(3) 0.0175(4) Uani 1 1 d .
C5 C 0.03602(14) 0.55524(9) 0.7818(2) 0.0169(4) Uani 1 1 d .
H5 H -0.0167 0.5485 0.8473 0.020 Uiso 1 1 calc R
C6 C 0.07460(13) 0.61383(8) 0.7794(2) 0.0136(4) Uani 1 1 d .
C7 C 0.27382(16) 0.58406(10) 0.4838(3) 0.0283(5) Uani 1 1 d .
H7A H 0.2597 0.6101 0.3874 0.042 Uiso 1 1 calc R
H7B H 0.2951 0.5440 0.4448 0.042 Uiso 1 1 calc R
H7C H 0.3212 0.6036 0.5513 0.042 Uiso 1 1 calc R
C8 C 0.03000(16) 0.44348(9) 0.6994(3) 0.0253(5) Uani 1 1 d .
H8A H 0.0110 0.4310 0.5871 0.038 Uiso 1 1 calc R
H8B H -0.0228 0.4444 0.7736 0.038 Uiso 1 1 calc R
H8C H 0.0745 0.4141 0.7426 0.038 Uiso 1 1 calc R
C9 C 0.03319(16) 0.66405(9) 0.8837(3) 0.0224(4) Uani 1 1 d .
H9A H 0.0678 0.7020 0.8685 0.034 Uiso 0.50 1 calc PR
H9B H 0.0345 0.6521 1.0018 0.034 Uiso 0.50 1 calc PR
H9C H -0.0297 0.6707 0.8488 0.034 Uiso 0.50 1 calc PR
H9D H -0.0194 0.6479 0.9443 0.034 Uiso 0.50 1 calc PR
H9E H 0.0139 0.6978 0.8109 0.034 Uiso 0.50 1 calc PR
H9F H 0.0781 0.6792 0.9640 0.034 Uiso 0.50 1 calc PR
C10 C 0.28424(16) 0.63890(10) 0.9207(3) 0.0245(5) Uani 1 1 d .
H10A H 0.2312 0.6202 0.9741 0.037 Uiso 1 1 calc R
H10B H 0.3262 0.6535 1.0069 0.037 Uiso 1 1 calc R
H10C H 0.3147 0.6084 0.8506 0.037 Uiso 1 1 calc R
C11 C 0.25413(12) 0.69242(8) 0.8135(2) 0.0125(4) Uani 1 1 d .
C12 C 0.28791(19) 0.7500 0.8599(3) 0.0138(5) Uani 1 2 d S
H12 H 0.3395 0.7500 0.9308 0.017 Uiso 1 2 calc SR
C13 C 0.03304(14) 0.71794(10) 0.4550(3) 0.0228(5) Uani 1 1 d .
H13 H -0.0007 0.6924 0.5283 0.027 Uiso 1 1 calc R
C14 C 0.09161(14) 0.69773(9) 0.3276(3) 0.0208(4) Uani 1 1 d .
H14 H 0.1051 0.6562 0.3008 0.025 Uiso 1 1 calc R
C15 C 0.1267(2) 0.7500 0.2471(4) 0.0208(6) Uani 1 2 d S
H15 H 0.1671 0.7500 0.1545 0.025 Uiso 1 2 calc SR
N1 N 0.19610(10) 0.68333(6) 0.68802(19) 0.0098(3) Uani 1 1 d .
Cr1 Cr 0.17384(3) 0.7500 0.51603(5) 0.00821(9) Uani 1 2 d S
I1 I 0.342147(12) 0.7500 0.38560(2) 0.01716(7) 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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
C2 C1 C6 120.23(17) . .
C2 C1 N1 120.96(17) . .
C6 C1 N1 118.75(16) . .
C1 C2 C3 118.62(18) . .
C1 C2 C7 122.00(18) . .
C3 C2 C7 119.36(17) . .
C4 C3 C2 122.46(18) . .
C4 C3 H3 118.8 . .
C2 C3 H3 118.8 . .
C3 C4 C5 117.66(17) . .
C3 C4 C8 121.27(18) . .
C5 C4 C8 121.07(19) . .
C4 C5 C6 122.28(18) . .
C4 C5 H5 118.9 . .
C6 C5 H5 118.9 . .
C5 C6 C1 118.73(17) . .
C5 C6 C9 119.39(18) . .
C1 C6 C9 121.85(17) . .
C2 C7 H7A 109.5 . .
C2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C4 C8 H8A 109.5 . .
C4 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C4 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C6 C9 H9D 109.5 . .
H9A C9 H9D 141.1 . .
H9B C9 H9D 56.3 . .
H9C C9 H9D 56.3 . .
C6 C9 H9E 109.5 . .
H9A C9 H9E 56.3 . .
H9B C9 H9E 141.1 . .
H9C C9 H9E 56.3 . .
H9D C9 H9E 109.5 . .
C6 C9 H9F 109.5 . .
H9A C9 H9F 56.3 . .
H9B C9 H9F 56.3 . .
H9C C9 H9F 141.1 . .
H9D C9 H9F 109.5 . .
H9E C9 H9F 109.5 . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N1 C11 C12 124.13(18) . .
N1 C11 C10 120.00(17) . .
C12 C11 C10 115.81(18) . .
C11 C12 C11 127.3(2) 8_575 .
C11 C12 H12 116.4 8_575 .
C11 C12 H12 116.4 . .
C13 C13 C14 108.25(12) 8_575 .
C13 C13 H13 125.9 8_575 .
C14 C13 H13 125.9 . .
C13 C14 C15 107.70(19) . .
C13 C14 H14 126.1 . .
C15 C14 H14 126.1 . .
C14 C15 C14 108.1(3) . 8_575
C14 C15 H15 126.0 . .
C14 C15 H15 126.0 8_575 .
C11 N1 C1 116.09(15) . .
C11 N1 Cr1 120.53(12) . .
C1 N1 Cr1 123.37(12) . .
N1 Cr1 N1 91.54(9) . 8_575
N1 Cr1 C14 155.02(7) . 8_575
N1 Cr1 C14 100.33(7) 8_575 8_575
N1 Cr1 C13 121.36(8) . 8_575
N1 Cr1 C13 94.28(7) 8_575 8_575
C14 Cr1 C13 36.50(8) 8_575 8_575
N1 Cr1 I1 96.51(5) . .
N1 Cr1 I1 96.51(5) 8_575 .
C14 Cr1 I1 103.79(6) 8_575 .
C13 Cr1 I1 140.24(6) 8_575 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.400(3) .
C1 C6 1.407(3) .
C1 N1 1.449(2) .
C2 C3 1.401(3) .
C2 C7 1.505(3) .
C3 C4 1.387(3) .
C3 H3 0.9500 .
C4 C5 1.389(3) .
C4 C8 1.511(3) .
C5 C6 1.398(3) .
C5 H5 0.9500 .
C6 C9 1.506(3) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C9 H9D 0.9800 .
C9 H9E 0.9800 .
C9 H9F 0.9800 .
C10 C11 1.515(3) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 N1 1.334(2) .
C11 C12 1.400(2) .
C12 C11 1.400(2) 8_575
C12 H12 0.9500 .
C13 C13 1.397(4) 8_575
C13 C14 1.407(3) .
C13 H13 0.9500 .
C14 C15 1.408(3) .
C14 H14 0.9500 .
C15 C14 1.408(3) 8_575
C15 H15 0.9500 .
N1 Cr1 2.0277(15) .
Cr1 N1 2.0277(15) 8_575
Cr1 C14 2.245(2) 8_575
Cr1 C13 2.246(2) 8_575
Cr1 I1 2.6941(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 -1.1(3) . .
N1 C1 C2 C3 176.02(17) . .
C6 C1 C2 C7 -179.58(19) . .
N1 C1 C2 C7 -2.5(3) . .
C1 C2 C3 C4 0.2(3) . .
C7 C2 C3 C4 178.8(2) . .
C2 C3 C4 C5 0.7(3) . .
C2 C3 C4 C8 -178.9(2) . .
C3 C4 C5 C6 -0.8(3) . .
C8 C4 C5 C6 178.82(19) . .
C4 C5 C6 C1 -0.1(3) . .
C4 C5 C6 C9 -178.39(19) . .
C2 C1 C6 C5 1.0(3) . .
N1 C1 C6 C5 -176.17(17) . .
C2 C1 C6 C9 179.27(19) . .
N1 C1 C6 C9 2.1(3) . .
N1 C11 C12 C11 15.4(4) . 8_575
C10 C11 C12 C11 -161.9(2) . 8_575
C13 C13 C14 C15 -0.94(19) 8_575 .
C13 C14 C15 C14 1.5(3) . 8_575
C12 C11 N1 C1 -166.3(2) . .
C10 C11 N1 C1 10.9(3) . .
C12 C11 N1 Cr1 14.8(3) . .
C10 C11 N1 Cr1 -168.01(15) . .
C2 C1 N1 C11 -92.8(2) . .
C6 C1 N1 C11 84.4(2) . .
C2 C1 N1 Cr1 86.1(2) . .
C6 C1 N1 Cr1 -96.74(19) . .
C11 N1 Cr1 N1 -31.48(17) . 8_575
C1 N1 Cr1 N1 149.68(11) . 8_575
C11 N1 Cr1 C14 -150.33(18) . 8_575
C1 N1 Cr1 C14 30.8(3) . 8_575
C11 N1 Cr1 C13 -127.43(14) . 8_575
C1 N1 Cr1 C13 53.73(16) . 8_575
C11 N1 Cr1 I1 65.26(14) . .
C1 N1 Cr1 I1 -113.59(13) . .
