#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:15:46 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178842 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/96/4109622.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_4109622
loop_
_publ_author_name
'Wesley H. Monillas'
'Glenn P. A. Yap'
'Leonard A. MacAdams'
'Klaus H. Theopold'
_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            'C68 H106 Cr2 N6'
_chemical_formula_weight         1111.59
_chemical_name_common            '[(i-Pr2Ph)2nacnacCr]2(N2)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 126.411(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.526(3)
_cell_length_b                   19.362(4)
_cell_length_c                   13.161(3)
_cell_measurement_reflns_used    745
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.58
_cell_measurement_theta_min      3.19
_cell_volume                     3389.1(12)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       ω
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9611
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.9312
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0496
_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/[σ²(Fo²)+(0.0697P)²+1.7701P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1419
_reflns_number_gt                3159
_reflns_number_total             3919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0725549si20070412_124410.cif
_cod_data_source_block           klat121
_cod_original_cell_volume        3389.0(11)
_cod_database_code               4109622
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.44065(3) 0.5000 0.32261(4) 0.02986(16) Uani 1 2 d S . .
N1 N 0.40363(12) 0.42525(8) 0.19395(14) 0.0299(4) Uani 1 1 d . . .
N2 N 0.5000 0.53225(12) 0.5000 0.0384(6) Uani 1 2 d S . .
C1 C 0.48088(17) 0.31640(11) 0.30650(19) 0.0382(5) Uani 1 1 d . . .
C2 C 0.4696(2) 0.25034(12) 0.3400(2) 0.0478(6) Uani 1 1 d . . .
H2A H 0.5276 0.2226 0.3942 0.057 Uiso 1 1 calc R . .
C3 C 0.3767(2) 0.22485(12) 0.2962(2) 0.0520(6) Uani 1 1 d . . .
H3A H 0.3709 0.1800 0.3205 0.062 Uiso 1 1 calc R . .
C4 C 0.2924(2) 0.26409(12) 0.2173(2) 0.0476(6) Uani 1 1 d . . .
H4A H 0.2285 0.2458 0.1872 0.057 Uiso 1 1 calc R . .
C5 C 0.29834(17) 0.33033(11) 0.18027(19) 0.0382(5) Uani 1 1 d . . .
C6 C 0.39399(15) 0.35589(10) 0.22618(17) 0.0318(4) Uani 1 1 d . . .
C7 C 0.58361(18) 0.34216(13) 0.3542(2) 0.0473(6) Uani 1 1 d . . .
H7A H 0.5761 0.3913 0.3263 0.057 Uiso 1 1 calc R . .
C8 C 0.6276(3) 0.3022(2) 0.2983(3) 0.0808(10) Uani 1 1 d . . .
H8A H 0.5825 0.3058 0.2060 0.121 Uiso 1 1 calc R . .
H8B H 0.6352 0.2535 0.3230 0.121 Uiso 1 1 calc R . .
H8C H 0.6935 0.3214 0.3297 0.121 Uiso 1 1 calc R . .
C9 C 0.6561(2) 0.34150(19) 0.4981(3) 0.0727(9) Uani 1 1 d . . .
H9A H 0.6254 0.3656 0.5329 0.109 Uiso 1 1 calc R . .
H9B H 0.7187 0.3649 0.5256 0.109 Uiso 1 1 calc R . .
H9C H 0.6708 0.2936 0.5282 0.109 Uiso 1 1 calc R . .
C10 C 0.20376(18) 0.37271(13) 0.0952(2) 0.0470(6) Uani 1 1 d . . .
H10A H 0.2199 0.4118 0.0604 0.056 Uiso 1 1 calc R . .
C11 C 0.1693(2) 0.40324(16) 0.1709(3) 0.0677(8) Uani 1 1 d . . .
H11A H 0.2244 0.4299 0.2421 0.102 Uiso 1 1 calc R . .
H11B H 0.1500 0.3658 0.2027 0.102 Uiso 1 1 calc R . .
H11C H 0.1114 0.4336 0.1163 0.102 Uiso 1 1 calc R . .
C12 C 0.1174(2) 0.33068(17) -0.0167(3) 0.0679(8) Uani 1 1 d . . .
H12A H 0.1412 0.3084 -0.0614 0.102 Uiso 1 1 calc R . .
H12B H 0.0613 0.3616 -0.0746 0.102 Uiso 1 1 calc R . .
H12C H 0.0949 0.2953 0.0147 0.102 Uiso 1 1 calc R . .
C13 C 0.3713(2) 0.37389(12) 0.0016(2) 0.0496(6) Uani 1 1 d . . .
H13A H 0.4198 0.3372 0.0531 0.074 Uiso 1 1 calc R . .
H13B H 0.3789 0.3882 -0.0638 0.074 Uiso 1 1 calc R . .
H13C H 0.3029 0.3566 -0.0383 0.074 Uiso 1 1 calc R . .
C14 C 0.39025(16) 0.43504(11) 0.08460(17) 0.0342(4) Uani 1 1 d . . .
C15 C 0.3890(2) 0.5000 0.0380(3) 0.0369(7) Uani 1 2 d S . .
H15A H 0.3869 0.5000 -0.0357 0.044 Uiso 1 2 calc SR . .
C16 C 0.7484(9) 0.5109(16) 0.3557(10) 0.176(9) Uani 0.50 1 d PD A -1
H16A H 0.7144 0.5495 0.2967 0.264 Uiso 0.50 1 calc PR A -1
H16B H 0.7023 0.4891 0.3698 0.264 Uiso 0.50 1 calc PR A -1
H16C H 0.7692 0.4768 0.3201 0.264 Uiso 0.50 1 calc PR A -1
C17 C 0.8298(12) 0.5343(7) 0.4660(12) 0.241(10) Uani 0.50 1 d PD A -1
H17A H 0.8631 0.5643 0.4399 0.289 Uiso 0.50 1 calc PR A -1
H17B H 0.8011 0.5665 0.4954 0.289 Uiso 0.50 1 calc PR A -1
C18 C 0.9073(7) 0.5055(16) 0.5733(9) 0.159(5) Uani 0.50 1 d PD A -1
H18A H 0.9355 0.4727 0.5441 0.190 Uiso 0.50 1 calc PR A -1
H18B H 0.8743 0.4763 0.6006 0.190 Uiso 0.50 1 calc PR A -1
C19 C 0.9920(11) 0.5306(7) 0.6864(11) 0.204(8) Uani 0.50 1 d PD A -1
H19A H 1.0219 0.5652 0.6623 0.244 Uiso 0.50 1 calc PR A -1
H19B H 0.9662 0.5568 0.7263 0.244 Uiso 0.50 1 calc PR A -1
C20 C 1.0715(9) 0.4920(15) 0.7818(10) 0.204(8) Uani 0.50 1 d PD A -1
H20A H 1.1226 0.5229 0.8484 0.306 Uiso 0.50 1 calc PR A -1
H20B H 1.1008 0.4652 0.7479 0.306 Uiso 0.50 1 calc PR A -1
H20C H 1.0475 0.4606 0.8170 0.306 Uiso 0.50 1 calc PR A -1
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'
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
N2 Cr1 N2 36.00(13) . 5_666
N2 Cr1 N1 116.32(7) . 6_565
N2 Cr1 N1 152.23(8) 5_666 6_565
N2 Cr1 N1 152.23(8) . .
N2 Cr1 N1 116.32(7) 5_666 .
N1 Cr1 N1 91.16(9) 6_565 .
C14 N1 C6 118.17(16) . .
C14 N1 Cr1 125.08(14) . .
C6 N1 Cr1 116.72(11) . .
N2 N2 Cr1 72.00(6) 5_666 .
N2 N2 Cr1 72.00(6) 5_666 5_666
Cr1 N2 Cr1 144.00(13) . 5_666
C6 C1 C2 117.9(2) . .
C6 C1 C7 122.1(2) . .
C2 C1 C7 120.0(2) . .
C3 C2 C1 121.4(2) . .
C4 C3 C2 120.0(2) . .
C3 C4 C5 121.5(2) . .
C4 C5 C6 117.9(2) . .
C4 C5 C10 120.0(2) . .
C6 C5 C10 122.08(19) . .
C1 C6 C5 121.32(19) . .
C1 C6 N1 119.11(18) . .
C5 C6 N1 119.53(18) . .
C1 C7 C8 112.1(2) . .
C1 C7 C9 112.1(2) . .
C8 C7 C9 110.4(2) . .
C5 C10 C11 110.4(2) . .
C5 C10 C12 112.6(2) . .
C11 C10 C12 109.6(2) . .
N1 C14 C15 123.55(19) . .
N1 C14 C13 119.91(18) . .
C15 C14 C13 116.49(18) . .
C14 C15 C14 128.9(2) . 6_565
C18 C17 C16 136(2) . .
C17 C18 C19 135(3) . .
C20 C19 C18 126.4(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N2 2.0209(9) .
Cr1 N2 2.0209(9) 5_666
Cr1 N1 2.0264(16) 6_565
Cr1 N1 2.0264(16) .
N1 C14 1.334(2) .
N1 C6 1.445(2) .
N2 N2 1.249(5) 5_666
N2 Cr1 2.0209(9) 5_666
C1 C6 1.401(3) .
C1 C2 1.401(3) .
C1 C7 1.503(3) .
C2 C3 1.372(4) .
C3 C4 1.371(4) .
C4 C5 1.396(3) .
C5 C6 1.405(3) .
C5 C10 1.514(3) .
C7 C8 1.518(4) .
C7 C9 1.526(3) .
C10 C11 1.529(4) .
C10 C12 1.540(3) .
C13 C14 1.512(3) .
C14 C15 1.394(2) .
C15 C14 1.394(2) 6_565
C16 C17 1.344(13) .
C17 C18 1.342(14) .
C18 C19 1.392(14) .
C19 C20 1.379(14) .
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
N2 Cr1 N1 C14 -156.68(13) . .
N2 Cr1 N1 C14 -160.57(15) 5_666 .
N1 Cr1 N1 C14 15.3(2) 6_565 .
N2 Cr1 N1 C6 21.5(2) . .
N2 Cr1 N1 C6 17.63(15) 5_666 .
N1 Cr1 N1 C6 -166.55(11) 6_565 .
N1 Cr1 N2 N2 -176.93(6) 6_565 5_666
N1 Cr1 N2 N2 -5.93(11) . 5_666
N2 Cr1 N2 Cr1 0.0 5_666 5_666
N1 Cr1 N2 Cr1 -176.93(6) 6_565 5_666
N1 Cr1 N2 Cr1 -5.93(11) . 5_666
C6 C1 C2 C3 -0.2(3) . .
C7 C1 C2 C3 -178.8(2) . .
C1 C2 C3 C4 0.4(3) . .
C2 C3 C4 C5 -0.4(3) . .
C3 C4 C5 C6 0.2(3) . .
C3 C4 C5 C10 -178.7(2) . .
C2 C1 C6 C5 0.0(3) . .
C7 C1 C6 C5 178.55(18) . .
C2 C1 C6 N1 177.60(17) . .
C7 C1 C6 N1 -3.8(3) . .
C4 C5 C6 C1 0.0(3) . .
C10 C5 C6 C1 178.92(19) . .
C4 C5 C6 N1 -177.59(17) . .
C10 C5 C6 N1 1.3(3) . .
C14 N1 C6 C1 97.6(2) . .
Cr1 N1 C6 C1 -80.76(19) . .
C14 N1 C6 C5 -84.7(2) . .
Cr1 N1 C6 C5 96.93(17) . .
C6 C1 C7 C8 -111.2(3) . .
C2 C1 C7 C8 67.3(3) . .
C6 C1 C7 C9 124.1(2) . .
C2 C1 C7 C9 -57.4(3) . .
C4 C5 C10 C11 77.4(3) . .
C6 C5 C10 C11 -101.5(2) . .
C4 C5 C10 C12 -45.4(3) . .
C6 C5 C10 C12 135.7(2) . .
C6 N1 C14 C15 174.3(2) . .
Cr1 N1 C14 C15 -7.6(3) . .
C6 N1 C14 C13 -3.3(3) . .
Cr1 N1 C14 C13 174.88(16) . .
N1 C14 C15 C14 -7.3(5) . 6_565
C13 C14 C15 C14 170.4(3) . 6_565
C16 C17 C18 C19 179(2) . .
C17 C18 C19 C20 -171.0(19) . .
