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#$Date: 2016-03-22 11:23:37 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178897 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/26/4112648.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_4112648
loop_
_publ_author_name
'John F. Berry'
'F. Albert Cotton'
'Tongbu Lu'
'Carlos A. Murillo'
'Brian K. Roberts'
'Xiaoping Wang'
_publ_contact_author_address
;  Laboratory for Molecular Structure and Bonding
   Dept. of Chemistry
   Texas A&M University, PO Box  30012
   College Station, TX 77842-3012, USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(979) 845 9351'
_publ_contact_author_name        'F. A. Cotton'
_publ_contact_author_phone       '(979) 845 4432'
_publ_section_title
;
 Molecular and Electronic Structures by Design: Tuning Symmetrical and
 Unsymmetrical Linear Trichromium Chains
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7082
_journal_page_last               7096
_journal_paper_doi               10.1021/ja049055h
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'Cr3(C10H8N3)4(NCS)2, 2(C6H6)'
_chemical_formula_sum            'C54 H44 Cr3 N14 S2'
_chemical_formula_weight         1109.15
_chemical_name_common            Cr3(dpa)4(NCS)2.2Benzene
_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                 108.149(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.956(6)
_cell_length_b                   18.688(6)
_cell_length_c                   16.949(6)
_cell_measurement_reflns_used    7577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     5103(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17808
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.9277
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'green black'
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       needle
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5802
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0463P)²+5.4985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4488
_reflns_number_total             5802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049055hsi20040409_043050_14.cif
_cod_data_source_block           10twobenzene
_cod_original_cell_volume        5104(3)
_cod_database_code               4112648
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 -0.090658(19) 0.184190(17) 0.33097(2) 0.02552(10) Uani 1 1 d .
N1 N -0.17666(10) 0.13182(9) 0.23069(11) 0.0267(4) Uani 1 1 d .
N1L N -0.17129(12) 0.18250(11) 0.41077(13) 0.0393(5) Uani 1 1 d .
N2 N -0.07051(10) 0.10738(9) 0.17640(10) 0.0250(3) Uani 1 1 d .
N3 N 0.04197(10) 0.08036(9) 0.13228(10) 0.0268(4) Uani 1 1 d .
N5 N -0.07133(10) 0.26099(9) 0.17618(10) 0.0248(3) Uani 1 1 d .
N6 N -0.00906(10) 0.23278(9) 0.07679(10) 0.0260(4) Uani 1 1 d .
N9 N -0.13443(10) 0.28365(9) 0.27600(11) 0.0275(4) Uani 1 1 d .
C1L C -0.20618(14) 0.15748(13) 0.45167(15) 0.0370(5) Uani 1 1 d .
C1A C 0.0207(2) 0.5098(3) 0.4295(3) 0.0849(13) Uani 1 1 d .
H1AA H 0.0351 0.5164 0.3814 0.102 Uiso 1 1 calc R
C1 C 0.0663(2) -0.23615(19) 0.3034(2) 0.110(2) Uani 1 1 d D
H1A H 0.1109 -0.2112 0.3386 0.132 Uiso 1 1 calc R
C2A C -0.02962(19) 0.4357(2) 0.5151(4) 0.0875(15) Uani 1 1 d .
H2AA H -0.0497 0.3917 0.5259 0.105 Uiso 1 1 calc R
C3A C -0.0096(2) 0.4452(2) 0.4448(3) 0.0823(12) Uani 1 1 d .
H3AA H -0.0163 0.4079 0.4069 0.099 Uiso 1 1 calc R
C5 C 0.0000 -0.3469(3) 0.2500 0.0853(17) Uani 1 2 d SD
H5A H 0.0000 -0.3967 0.2500 0.102 Uiso 1 2 calc SR
C6 C 0.06608(19) -0.31035(19) 0.3043(2) 0.0928(14) Uani 1 1 d D
H6A H 0.1097 -0.3354 0.3409 0.111 Uiso 1 1 calc R
C11 C -0.15273(12) 0.10003(10) 0.16984(13) 0.0264(4) Uani 1 1 d .
C12 C -0.21263(14) 0.06505(12) 0.10364(15) 0.0350(5) Uani 1 1 d .
H12A H -0.1974 0.0464 0.0596 0.042 Uiso 1 1 calc R
C13 C -0.29303(14) 0.05873(13) 0.10439(16) 0.0418(6) Uani 1 1 d .
H13A H -0.3319 0.0342 0.0621 0.050 Uiso 1 1 calc R
C14 C -0.31594(14) 0.08921(14) 0.16867(16) 0.0414(6) Uani 1 1 d .
H14A H -0.3698 0.0846 0.1710 0.050 Uiso 1 1 calc R
C15 C -0.25697(13) 0.12626(12) 0.22865(15) 0.0340(5) Uani 1 1 d .
H15A H -0.2729 0.1488 0.2702 0.041 Uiso 1 1 calc R
C31 C -0.02961(12) 0.05724(11) 0.14424(12) 0.0263(4) Uani 1 1 d .
C32 C -0.05279(14) -0.01527(12) 0.13112(14) 0.0348(5) Uani 1 1 d .
H32A H -0.1011 -0.0313 0.1403 0.042 Uiso 1 1 calc R
C33 C -0.00398(16) -0.06223(12) 0.10482(16) 0.0411(6) Uani 1 1 d .
H33A H -0.0196 -0.1100 0.0954 0.049 Uiso 1 1 calc R
C34 C 0.06865(16) -0.03837(12) 0.09229(16) 0.0395(5) Uani 1 1 d .
H34A H 0.1023 -0.0694 0.0742 0.047 Uiso 1 1 calc R
C35 C 0.08932(14) 0.03232(12) 0.10742(14) 0.0334(5) Uani 1 1 d .
H35A H 0.1386 0.0483 0.1002 0.040 Uiso 1 1 calc R
C61 C -0.07690(12) 0.25925(10) 0.09364(13) 0.0258(4) Uani 1 1 d .
C62 C -0.14860(14) 0.27712(12) 0.02822(14) 0.0340(5) Uani 1 1 d .
H62A H -0.1949 0.2950 0.0400 0.041 Uiso 1 1 calc R
C63 C -0.15076(15) 0.26844(13) -0.05244(15) 0.0389(5) Uani 1 1 d .
H63A H -0.1991 0.2779 -0.0956 0.047 Uiso 1 1 calc R
C64 C -0.07979(16) 0.24532(13) -0.06923(14) 0.0406(6) Uani 1 1 d .
H64A H -0.0787 0.2414 -0.1236 0.049 Uiso 1 1 calc R
C65 C -0.01155(14) 0.22841(12) -0.00362(14) 0.0332(5) Uani 1 1 d .
H65A H 0.0359 0.2130 -0.0150 0.040 Uiso 1 1 calc R
C91 C -0.11920(12) 0.30616(11) 0.20598(13) 0.0268(4) Uani 1 1 d .
C92 C -0.14800(14) 0.37395(12) 0.17185(16) 0.0368(5) Uani 1 1 d .
H92A H -0.1357 0.3902 0.1252 0.044 Uiso 1 1 calc R
C93 C -0.19396(17) 0.41558(14) 0.20766(17) 0.0462(6) Uani 1 1 d .
H93A H -0.2132 0.4601 0.1852 0.055 Uiso 1 1 calc R
C94 C -0.21167(17) 0.39113(14) 0.27749(18) 0.0469(6) Uani 1 1 d .
H94A H -0.2443 0.4180 0.3016 0.056 Uiso 1 1 calc R
C95 C -0.17977(14) 0.32622(12) 0.31007(16) 0.0369(5) Uani 1 1 d .
H95A H -0.1898 0.3106 0.3581 0.044 Uiso 1 1 calc R
S1L S -0.25542(6) 0.11934(5) 0.50862(6) 0.0737(3) Uani 1 1 d .
C2 C 0.0000 -0.1991(3) 0.2500 0.119(3) Uani 1 2 d SD
H2A H 0.0000 -0.1493 0.2500 0.143 Uiso 1 2 calc SR
Cr2 Cr -0.00481(8) 0.18490(2) 0.25422(8) 0.02119(15) Uiso 0.50 1 d P
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'
S S 0.1246 0.1234 '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 Cr1 N9 89.61(7) . .
N1 Cr1 N6 171.53(6) . 2
N9 Cr1 N6 92.20(7) . 2
N1 Cr1 N3 85.43(7) . 2
N9 Cr1 N3 170.43(7) . 2
N6 Cr1 N3 91.56(7) 2 2
N1 Cr1 N1L 94.74(8) . .
N9 Cr1 N1L 94.80(7) . .
N6 Cr1 N1L 93.35(7) 2 .
N3 Cr1 N1L 93.77(7) 2 .
N1 Cr1 Cr2 86.89(6) . .
N9 Cr1 Cr2 86.62(5) . .
N6 Cr1 Cr2 84.96(6) 2 .
N3 Cr1 Cr2 84.95(5) 2 .
N1L Cr1 Cr2 177.84(7) . .
N1 Cr1 Cr2 86.91(6) . 2
N9 Cr1 Cr2 86.66(5) . 2
N6 Cr1 Cr2 84.93(6) 2 2
N3 Cr1 Cr2 84.90(5) 2 2
N1L Cr1 Cr2 177.79(7) . 2
C15 N1 C11 118.87(18) . .
C15 N1 Cr1 119.62(15) . .
C11 N1 Cr1 121.42(13) . .
C1L N1L Cr1 156.4(2) . .
C11 N2 C31 121.69(17) . .
C11 N2 Cr2 117.41(13) . .
C31 N2 Cr2 119.91(13) . .
C11 N2 Cr2 123.74(13) . 2
C31 N2 Cr2 114.14(13) . 2
C35 N3 C31 118.53(18) . .
C35 N3 Cr1 118.82(14) . 2
C31 N3 Cr1 121.94(13) . 2
C91 N5 C61 121.94(17) . .
C91 N5 Cr2 117.64(14) . .
C61 N5 Cr2 119.72(13) . .
C91 N5 Cr2 123.95(14) . 2
C61 N5 Cr2 113.86(13) . 2
C65 N6 C61 118.04(18) . .
C65 N6 Cr1 119.02(14) . 2
C61 N6 Cr1 122.24(13) . 2
C95 N9 C91 118.59(19) . .
C95 N9 Cr1 119.87(15) . .
C91 N9 Cr1 121.53(13) . .
N1L C1L S1L 178.1(2) . .
C2A C1A C3A 119.8(4) 5_566 .
C6 C1 C2 120.1(4) . .
C3A C2A C1A 120.4(4) . 5_566
C2A C3A C1A 119.7(4) . .
C6 C5 C6 121.0(5) . 2
C1 C6 C5 119.3(4) . .
N1 C11 N2 115.58(18) . .
N1 C11 C12 119.57(19) . .
N2 C11 C12 124.79(19) . .
C13 C12 C11 120.1(2) . .
C12 C13 C14 119.6(2) . .
C15 C14 C13 118.1(2) . .
N1 C15 C14 123.6(2) . .
N3 C31 N2 115.20(17) . .
N3 C31 C32 119.95(18) . .
N2 C31 C32 124.57(19) . .
C33 C32 C31 120.0(2) . .
C32 C33 C34 119.9(2) . .
C35 C34 C33 118.0(2) . .
N3 C35 C34 123.7(2) . .
N6 C61 N5 115.34(17) . .
N6 C61 C62 119.99(19) . .
N5 C61 C62 124.46(19) . .
C63 C62 C61 120.5(2) . .
C62 C63 C64 119.2(2) . .
C65 C64 C63 118.2(2) . .
N6 C65 C64 123.9(2) . .
N9 C91 N5 115.25(18) . .
N9 C91 C92 119.96(19) . .
N5 C91 C92 124.67(19) . .
C93 C92 C91 119.9(2) . .
C92 C93 C94 119.7(2) . .
C95 C94 C93 118.2(2) . .
N9 C95 C94 123.6(2) . .
C1 C2 C1 120.2(6) 2 .
Cr2 Cr2 N5 87.5(5) 2 .
Cr2 Cr2 N5 85.5(5) 2 2
N5 Cr2 N5 90.67(10) . 2
Cr2 Cr2 N2 87.2(5) 2 .
N5 Cr2 N2 89.74(9) . .
N5 Cr2 N2 172.73(9) 2 .
Cr2 Cr2 N2 85.8(4) 2 2
N5 Cr2 N2 173.22(9) . 2
N5 Cr2 N2 89.53(9) 2 2
N2 Cr2 N2 89.21(10) . 2
Cr2 Cr2 Cr1 179.5(6) 2 .
N5 Cr2 Cr1 93.04(6) . .
N5 Cr2 Cr1 94.44(7) 2 .
N2 Cr2 Cr1 92.79(6) . .
N2 Cr2 Cr1 93.70(7) 2 .
N5 Cr2 Cr1 87.44(6) . 2
N5 Cr2 Cr1 85.98(6) 2 2
N2 Cr2 Cr1 86.78(6) . 2
N2 Cr2 Cr1 85.82(6) 2 2
Cr1 Cr2 Cr1 179.35(3) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N1 2.1045(18) .
Cr1 N9 2.1079(18) .
Cr1 N6 2.1169(18) 2
Cr1 N3 2.1246(18) 2
Cr1 N1L 2.203(2) .
Cr1 Cr2 2.2341(13) .
Cr1 Cr2 2.4823(13) 2
N1 C15 1.355(3) .
N1 C11 1.357(3) .
N1L C1L 1.142(3) .
N2 C11 1.371(3) .
N2 C31 1.375(3) .
N2 Cr2 2.041(2) .
N2 Cr2 2.0437(19) 2
N3 C35 1.356(3) .
N3 C31 1.362(3) .
N3 Cr1 2.1246(18) 2
N5 C91 1.372(3) .
N5 C61 1.373(3) .
N5 Cr2 2.028(2) .
N5 Cr2 2.033(2) 2
N6 C65 1.353(3) .
N6 C61 1.362(3) .
N6 Cr1 2.1169(18) 2
N9 C95 1.354(3) .
N9 C91 1.358(3) .
C1L S1L 1.624(2) .
C1A C2A 1.361(6) 5_566
C1A C3A 1.368(5) .
C1 C6 1.3867(11) .
C1 C2 1.3891(7) .
C2A C3A 1.349(6) .
C2A C1A 1.361(6) 5_566
C5 C6 1.3881(8) .
C5 C6 1.3881(8) 2
C11 C12 1.417(3) .
C12 C13 1.372(3) .
C13 C14 1.388(4) .
C14 C15 1.371(3) .
C31 C32 1.409(3) .
C32 C33 1.372(3) .
C33 C34 1.387(3) .
C34 C35 1.370(3) .
C61 C62 1.407(3) .
C62 C63 1.366(3) .
C63 C64 1.389(3) .
C64 C65 1.369(3) .
C91 C92 1.415(3) .
C92 C93 1.370(3) .
C93 C94 1.386(4) .
C94 C95 1.372(3) .
C2 C1 1.3891(7) 2
Cr2 N5 2.033(2) 2
Cr2 N2 2.0437(19) 2
Cr2 Cr1 2.4823(13) 2
