#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:29:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178872 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/01/4110187.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_4110187
loop_
_publ_author_name
'Kevin A. Kreisel'
'Glenn P. A. Yap'
'Olga Dmitrenko'
'Clark R. Landis'
'Klaus H. Theopold'
_publ_section_title
;
 The Shortest Metal-Metal Bond Yet: Molecular and Electronic Structure of
 a Dinuclear Chromium Diazadiene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14162
_journal_page_last               14163
_journal_paper_doi               10.1021/ja076356t
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C52 H72 Cr2 N4'
_chemical_formula_weight         857.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.718(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.387(8)
_cell_length_b                   9.742(3)
_cell_length_c                   24.917(7)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.32
_cell_volume                     5013(3)
_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      293(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22268
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_correction_T_min  0.8613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.816
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0470
_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)+(0.0625P)²+10.3564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1282
_reflns_number_gt                3813
_reflns_number_total             4410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja076356tsi20070930_113023.cif
_cod_data_source_block           klat395a
_cod_database_code               4110187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Cr1 Cr 0.469992(18) 0.13785(4) 0.213316(16) 0.02358(14) Uani 1 1 d .
N1 N 0.44370(9) -0.0499(2) 0.19784(8) 0.0249(4) Uani 1 1 d .
N2 N 0.46287(10) 0.3260(2) 0.18974(8) 0.0253(4) Uani 1 1 d .
C1 C 0.32806(12) -0.0880(3) 0.17357(12) 0.0330(6) Uani 1 1 d .
C2 C 0.26603(13) -0.1151(3) 0.13174(14) 0.0427(7) Uani 1 1 d .
H2A H 0.2316 -0.1259 0.1435 0.051 Uiso 1 1 calc R
C3 C 0.25521(13) -0.1258(3) 0.07405(14) 0.0448(8) Uani 1 1 d .
H3A H 0.2139 -0.1455 0.0471 0.054 Uiso 1 1 calc R
C4 C 0.30529(14) -0.1077(3) 0.05580(13) 0.0422(7) Uani 1 1 d .
H4A H 0.2971 -0.1139 0.0163 0.051 Uiso 1 1 calc R
C5 C 0.36841(12) -0.0800(3) 0.09532(11) 0.0323(6) Uani 1 1 d .
C6 C 0.37892(11) -0.0722(2) 0.15449(11) 0.0276(5) Uani 1 1 d .
C7 C 0.33873(14) -0.0754(3) 0.23751(13) 0.0406(7) Uani 1 1 d .
H7A H 0.3851 -0.0602 0.2594 0.049 Uiso 1 1 calc R
C8 C 0.3206(3) -0.2061(4) 0.26072(19) 0.0863(14) Uani 1 1 d .
H8A H 0.3440 -0.2820 0.2538 0.129 Uiso 1 1 calc R
H8B H 0.2749 -0.2220 0.2413 0.129 Uiso 1 1 calc R
H8C H 0.3314 -0.1969 0.3018 0.129 Uiso 1 1 calc R
C9 C 0.30354(19) 0.0473(4) 0.24770(17) 0.0658(10) Uani 1 1 d .
H9A H 0.3198 0.1294 0.2368 0.099 Uiso 1 1 calc R
H9B H 0.3104 0.0521 0.2881 0.099 Uiso 1 1 calc R
H9C H 0.2581 0.0387 0.2247 0.099 Uiso 1 1 calc R
C10 C 0.42374(15) -0.0653(3) 0.07489(12) 0.0436(7) Uani 1 1 d .
H10A H 0.4566 -0.0070 0.1031 0.052 Uiso 1 1 calc R
C11 C 0.40424(18) 0.0029(4) 0.01570(14) 0.0559(9) Uani 1 1 d .
H11A H 0.3837 0.0892 0.0160 0.084 Uiso 1 1 calc R
H11B H 0.3746 -0.0555 -0.0136 0.084 Uiso 1 1 calc R
H11C H 0.4421 0.0181 0.0072 0.084 Uiso 1 1 calc R
C12 C 0.4551(2) -0.2058(5) 0.07511(18) 0.0770(13) Uani 1 1 d .
H12A H 0.4723 -0.2418 0.1140 0.116 Uiso 1 1 calc R
H12B H 0.4895 -0.1955 0.0614 0.116 Uiso 1 1 calc R
H12C H 0.4232 -0.2678 0.0501 0.116 Uiso 1 1 calc R
C13 C 0.47267(12) -0.1682(3) 0.22583(12) 0.0324(6) Uani 1 1 d .
H13A H 0.4537 -0.2519 0.2107 0.039 Uiso 1 1 calc R
C14 C 0.36664(12) 0.3617(3) 0.09914(11) 0.0300(6) Uani 1 1 d .
C15 C 0.34080(14) 0.3840(3) 0.03919(11) 0.0371(6) Uani 1 1 d .
H15A H 0.2963 0.3940 0.0197 0.044 Uiso 1 1 calc R
C16 C 0.38047(14) 0.3913(3) 0.00853(11) 0.0381(6) Uani 1 1 d .
H16A H 0.3625 0.4064 -0.0314 0.046 Uiso 1 1 calc R
C17 C 0.44676(14) 0.3764(3) 0.03665(11) 0.0378(6) Uani 1 1 d .
H17A H 0.4729 0.3819 0.0154 0.045 Uiso 1 1 calc R
C18 C 0.47508(13) 0.3532(3) 0.09672(11) 0.0312(6) Uani 1 1 d .
C19 C 0.43414(12) 0.3464(2) 0.12725(10) 0.0265(5) Uani 1 1 d .
C20 C 0.32234(13) 0.3614(3) 0.13254(12) 0.0390(7) Uani 1 1 d .
H20A H 0.3469 0.3253 0.1716 0.047 Uiso 1 1 calc R
C21 C 0.26235(14) 0.2719(3) 0.10416(13) 0.0445(7) Uani 1 1 d .
H21A H 0.2753 0.1811 0.0982 0.067 Uiso 1 1 calc R
H21B H 0.2354 0.3108 0.0674 0.067 Uiso 1 1 calc R
H21C H 0.2386 0.2674 0.1290 0.067 Uiso 1 1 calc R
C22 C 0.3019(2) 0.5104(4) 0.1388(2) 0.0722(12) Uani 1 1 d .
H22A H 0.3398 0.5654 0.1578 0.108 Uiso 1 1 calc R
H22B H 0.2757 0.5105 0.1616 0.108 Uiso 1 1 calc R
H22C H 0.2774 0.5476 0.1010 0.108 Uiso 1 1 calc R
C23 C 0.54886(13) 0.3417(3) 0.12755(12) 0.0380(6) Uani 1 1 d .
H23A H 0.5583 0.3076 0.1670 0.046 Uiso 1 1 calc R
C24 C 0.57742(16) 0.2404(4) 0.09774(16) 0.0614(10) Uani 1 1 d .
H24A H 0.5567 0.1529 0.0948 0.092 Uiso 1 1 calc R
H24B H 0.6230 0.2311 0.1201 0.092 Uiso 1 1 calc R
H24C H 0.5706 0.2733 0.0595 0.092 Uiso 1 1 calc R
C25 C 0.58094(16) 0.4831(4) 0.13311(18) 0.0645(10) Uani 1 1 d .
H25A H 0.6267 0.4746 0.1551 0.097 Uiso 1 1 calc R
H25B H 0.5627 0.5450 0.1527 0.097 Uiso 1 1 calc R
H25C H 0.5735 0.5181 0.0950 0.097 Uiso 1 1 calc R
C26 C 0.48300(15) 0.4440(3) 0.22087(11) 0.0383(7) Uani 1 1 d .
H26A H 0.4730 0.5276 0.2014 0.046 Uiso 1 1 calc R
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
Cr1 Cr1 N2 104.63(6) 2_655
Cr1 Cr1 N1 104.78(6) 2_655
N2 Cr1 N1 150.58(9) .
C13 N1 C6 113.1(2) .
C13 N1 Cr1 130.64(17) .
C6 N1 Cr1 115.71(15) .
C26 N2 C19 114.0(2) .
C26 N2 Cr1 131.60(17) .
C19 N2 Cr1 114.26(15) .
C6 C1 C2 118.0(3) .
C6 C1 C7 121.8(2) .
C2 C1 C7 120.2(3) .
C3 C2 C1 121.2(3) .
C2 C3 C4 120.2(3) .
C3 C4 C5 121.5(3) .
C4 C5 C6 117.6(3) .
C4 C5 C10 121.0(3) .
C6 C5 C10 121.4(2) .
C1 C6 C5 121.5(2) .
C1 C6 N1 118.2(2) .
C5 C6 N1 120.3(2) .
C9 C7 C8 111.5(3) .
C9 C7 C1 111.1(3) .
C8 C7 C1 112.0(3) .
C5 C10 C11 113.6(3) .
C5 C10 C12 110.3(3) .
C11 C10 C12 110.6(3) .
C13 C13 N1 122.86(14) 2_655
C15 C14 C19 118.1(2) .
C15 C14 C20 119.9(2) .
C19 C14 C20 122.0(2) .
C16 C15 C14 120.8(3) .
C15 C16 C17 120.6(2) .
C16 C17 C18 120.8(3) .
C19 C18 C17 117.9(2) .
C19 C18 C23 121.9(2) .
C17 C18 C23 120.2(2) .
C18 C19 C14 121.8(2) .
C18 C19 N2 118.5(2) .
C14 C19 N2 119.6(2) .
C14 C20 C21 113.0(2) .
C14 C20 C22 109.6(3) .
C21 C20 C22 109.9(3) .
C24 C23 C18 112.2(2) .
C24 C23 C25 110.9(3) .
C18 C23 C25 110.8(2) .
C26 C26 N2 122.39(14) 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 Cr1 1.8028(9) 2_655
Cr1 N2 1.913(2) .
Cr1 N1 1.914(2) .
N1 C13 1.373(3) .
N1 C6 1.452(3) .
N2 C26 1.362(3) .
N2 C19 1.451(3) .
C1 C6 1.401(4) .
C1 C2 1.402(4) .
C1 C7 1.522(4) .
C2 C3 1.366(5) .
C3 C4 1.374(5) .
C4 C5 1.402(4) .
C5 C6 1.403(4) .
C5 C10 1.517(4) .
C7 C9 1.506(5) .
C7 C8 1.517(5) .
C10 C11 1.520(4) .
C10 C12 1.537(5) .
C13 C13 1.345(5) 2_655
C14 C15 1.395(4) .
C14 C19 1.407(4) .
C14 C20 1.521(4) .
C15 C16 1.379(4) .
C16 C17 1.382(4) .
C17 C18 1.400(4) .
C18 C19 1.401(4) .
C18 C23 1.533(4) .
C20 C21 1.527(4) .
C20 C22 1.548(5) .
C23 C24 1.517(4) .
C23 C25 1.534(4) .
C26 C26 1.354(5) 2_655
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
Cr1 Cr1 N1 C13 -16.9(2) 2_655 .
N2 Cr1 N1 C13 165.0(2) . .
Cr1 Cr1 N1 C6 154.00(16) 2_655 .
N2 Cr1 N1 C6 -24.1(3) . .
Cr1 Cr1 N2 C26 -15.3(3) 2_655 .
N1 Cr1 N2 C26 162.8(2) . .
Cr1 Cr1 N2 C19 160.70(15) 2_655 .
N1 Cr1 N2 C19 -21.2(3) . .
C6 C1 C2 C3 0.0(4) . .
C7 C1 C2 C3 179.5(3) . .
C1 C2 C3 C4 -1.2(4) . .
C2 C3 C4 C5 1.0(4) . .
C3 C4 C5 C6 0.4(4) . .
C3 C4 C5 C10 177.7(3) . .
C2 C1 C6 C5 1.4(4) . .
C7 C1 C6 C5 -178.1(2) . .
C2 C1 C6 N1 -177.4(2) . .
C7 C1 C6 N1 3.0(4) . .
C4 C5 C6 C1 -1.6(4) . .
C10 C5 C6 C1 -178.9(3) . .
C4 C5 C6 N1 177.2(2) . .
C10 C5 C6 N1 -0.1(4) . .
C13 N1 C6 C1 78.3(3) . .
Cr1 N1 C6 C1 -94.2(2) . .
C13 N1 C6 C5 -100.5(3) . .
Cr1 N1 C6 C5 87.0(2) . .
C6 C1 C7 C9 114.3(3) . .
C2 C1 C7 C9 -65.2(4) . .
C6 C1 C7 C8 -120.2(3) . .
C2 C1 C7 C8 60.3(4) . .
C4 C5 C10 C11 35.7(4) . .
C6 C5 C10 C11 -147.0(3) . .
C4 C5 C10 C12 -89.2(3) . .
C6 C5 C10 C12 88.1(3) . .
C6 N1 C13 C13 -167.8(3) . 2_655
Cr1 N1 C13 C13 3.3(5) . 2_655
C19 C14 C15 C16 -0.3(4) . .
C20 C14 C15 C16 176.8(3) . .
C14 C15 C16 C17 0.1(4) . .
C15 C16 C17 C18 0.2(4) . .
C16 C17 C18 C19 -0.4(4) . .
C16 C17 C18 C23 -178.0(3) . .
C17 C18 C19 C14 0.2(4) . .
C23 C18 C19 C14 177.8(2) . .
C17 C18 C19 N2 -178.4(2) . .
C23 C18 C19 N2 -0.9(4) . .
C15 C14 C19 C18 0.1(4) . .
C20 C14 C19 C18 -176.9(2) . .
C15 C14 C19 N2 178.7(2) . .
C20 C14 C19 N2 1.7(4) . .
C26 N2 C19 C18 85.2(3) . .
Cr1 N2 C19 C18 -91.5(2) . .
C26 N2 C19 C14 -93.5(3) . .
Cr1 N2 C19 C14 89.8(2) . .
C15 C14 C20 C21 48.6(4) . .
C19 C14 C20 C21 -134.5(3) . .
C15 C14 C20 C22 -74.3(3) . .
C19 C14 C20 C22 102.6(3) . .
C19 C18 C23 C24 131.7(3) . .
C17 C18 C23 C24 -50.8(4) . .
C19 C18 C23 C25 -103.6(3) . .
C17 C18 C23 C25 73.9(3) . .
C19 N2 C26 C26 -172.9(4) . 2_655
Cr1 N2 C26 C26 3.1(6) . 2_655
