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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/4/11/26/4112641.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_4112641
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(C14H16N3)4Cl2I3
_chemical_formula_sum            'C56 H64 Cl2 Cr3 I3 N12'
_chemical_formula_weight         1512.79
_chemical_name_common            '[Cr3(depa)4Cl2]I3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           120
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 -2c'
_symmetry_space_group_name_H-M   'I -4 c 2'
_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                   17.9292(12)
_cell_length_b                   17.9292(12)
_cell_length_c                   21.828(3)
_cell_measurement_reflns_used    8530
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     7016.7(12)
_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 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11129
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         10.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_T_max  0.6290
_exptl_absorpt_correction_T_min  0.5332
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'green black'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0984
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1142P)²+95.1017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2526
_refine_ls_wR_factor_ref         0.2588
_reflns_number_gt                1899
_reflns_number_total             2026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049055hsi20040409_043050_07.cif
_cod_data_source_block           3
_cod_original_cell_volume        7016.8(11)
_cod_database_code               4112641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
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 0.59045(9) 0.09045(9) 0.5000 0.0403(8) Uani 1 2 d S . .
Cr2 Cr 0.5058(3) 0.0058(3) 0.5000 0.0361(12) Uiso 0.50 2 d SP . .
N1 N 0.5100(5) 0.1598(5) 0.4616(5) 0.043(2) Uani 1 1 d . A .
N2 N 0.4201(4) 0.0799(4) 0.5000 0.034(3) Uani 1 2 d S . .
N3 N 0.6179(6) 0.0504(5) 0.4112(5) 0.042(2) Uani 1 1 d . B .
N4 N 0.5000 0.0000 0.4075(5) 0.036(3) Uani 1 2 d S . .
C11 C 0.4342(7) 0.1418(6) 0.4697(6) 0.044(3) Uani 1 1 d . . .
C12 C 0.3791(7) 0.1877(8) 0.4418(6) 0.048(3) Uani 1 1 d . A .
H12A H 0.3284 0.1754 0.4464 0.057 Uiso 1 1 calc R . .
C13 C 0.3987(8) 0.2500(7) 0.4081(6) 0.052(3) Uani 1 1 d D . .
C14 C 0.4740(9) 0.2680(7) 0.4031(6) 0.054(4) Uani 1 1 d . A .
H14A H 0.4884 0.3118 0.3825 0.065 Uiso 1 1 calc R . .
C15 C 0.5271(7) 0.2222(7) 0.4280(7) 0.047(3) Uani 1 1 d . . .
H15A H 0.5776 0.2341 0.4219 0.057 Uiso 1 1 calc R A .
C31 C 0.5670(6) 0.0122(6) 0.3798(5) 0.035(3) Uani 1 1 d . . .
C32 C 0.5859(8) -0.0202(7) 0.3225(6) 0.049(3) Uani 1 1 d . B .
H32A H 0.5498 -0.0472 0.3005 0.058 Uiso 1 1 calc R . .
C33 C 0.6566(7) -0.0125(7) 0.2990(6) 0.046(3) Uani 1 1 d . . .
C34 C 0.7082(7) 0.0271(8) 0.3333(7) 0.055(3) Uani 1 1 d . B .
H34A H 0.7570 0.0333 0.3185 0.066 Uiso 1 1 calc R . .
C35 C 0.6885(8) 0.0572(7) 0.3885(6) 0.048(3) Uani 1 1 d . . .
H35A H 0.7246 0.0832 0.4114 0.058 Uiso 1 1 calc R B .
C131 C 0.345(2) 0.3079(17) 0.3860(19) 0.070 Uiso 0.51(4) 1 d PD A 1
C132 C 0.359(3) 0.389(2) 0.366(2) 0.100 Uiso 0.51(4) 1 d PD A 1
C13A C 0.339(2) 0.292(2) 0.3736(17) 0.070 Uiso 0.49(4) 1 d PD A 2
H13C H 0.3576 0.3404 0.3596 0.084 Uiso 1 1 calc R A 2
H13D H 0.2950 0.2998 0.3994 0.084 Uiso 1 1 calc R A 2
C13' C 0.319(3) 0.239(3) 0.317(2) 0.100 Uiso 0.49(4) 1 d PD A 2
H13H H 0.2806 0.2626 0.2922 0.150 Uiso 1 1 calc R A 2
H13I H 0.3019 0.1915 0.3315 0.150 Uiso 1 1 calc R A 2
H13J H 0.3636 0.2323 0.2917 0.150 Uiso 1 1 calc R A 2
C331 C 0.6774(9) -0.0486(9) 0.2403(8) 0.061(4) Uiso 0.41(4) 1 d P B 1
H33A H 0.7128 -0.0164 0.2187 0.073 Uiso 0.41(4) 1 calc PR B 1
H33B H 0.6327 -0.0531 0.2148 0.073 Uiso 0.41(4) 1 calc PR B 1
C332 C 0.712(4) -0.124(4) 0.248(3) 0.100 Uiso 0.41(4) 1 d P B 1
H33E H 0.7243 -0.1445 0.2078 0.150 Uiso 0.41(4) 1 calc PR B 1
H33F H 0.6764 -0.1574 0.2679 0.150 Uiso 0.41(4) 1 calc PR B 1
H33G H 0.7565 -0.1205 0.2724 0.150 Uiso 0.41(4) 1 calc PR B 1
C33A C 0.6774(9) -0.0486(9) 0.2403(8) 0.061(4) Uiso 0.59(4) 1 d P B 2
H33C H 0.6805 -0.0101 0.2086 0.073 Uiso 0.59(4) 1 calc PR B 2
H33D H 0.6374 -0.0831 0.2286 0.073 Uiso 0.59(4) 1 calc PR B 2
C33' C 0.754(3) -0.093(3) 0.241(2) 0.100 Uiso 0.59(4) 1 d P B 2
H33H H 0.7636 -0.1135 0.2007 0.150 Uiso 0.59(4) 1 calc PR B 2
H33I H 0.7507 -0.1339 0.2705 0.150 Uiso 0.59(4) 1 calc PR B 2
H33J H 0.7941 -0.0601 0.2527 0.150 Uiso 0.59(4) 1 calc PR B 2
Cl1 Cl 0.68336(14) 0.18336(14) 0.5000 0.0538(12) Uani 1 2 d S . .
I1 I 0.5251(3) 0.4366(4) 0.2483(4) 0.118(2) Uani 0.25 1 d PU . .
I2 I 0.4367(2) 0.5198(2) 0.3435(2) 0.0650(11) Uani 0.25 1 d PU . .
I3 I 0.3465(3) 0.5894(4) 0.4345(3) 0.108(2) Uani 0.25 1 d PU . .
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'
Cl Cl 0.1484 0.1585 '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
N1 Cr1 N1 172.2(6) 15_545 .
N1 Cr1 N3 89.7(4) 15_545 .
N1 Cr1 N3 89.7(4) . .
N1 Cr1 N3 89.7(4) 15_545 15_545
N1 Cr1 N3 89.7(4) . 15_545
N3 Cr1 N3 171.4(6) . 15_545
N1 Cr1 Cr2 86.1(3) 15_545 .
N1 Cr1 Cr2 86.1(3) . .
N3 Cr1 Cr2 85.7(3) . .
N3 Cr1 Cr2 85.7(3) 15_545 .
N1 Cr1 Cl1 93.9(3) 15_545 .
N1 Cr1 Cl1 93.9(3) . .
N3 Cr1 Cl1 94.3(3) . .
N3 Cr1 Cl1 94.3(3) 15_545 .
Cr2 Cr1 Cl1 180.0(3) . .
N1 Cr1 Cr2 86.1(3) 15_545 2_655
N1 Cr1 Cr2 86.1(3) . 2_655
N3 Cr1 Cr2 85.7(3) . 2_655
N3 Cr1 Cr2 85.7(3) 15_545 2_655
Cl1 Cr1 Cr2 180.0 . 2_655
Cr2 Cr2 N4 85.8(2) 2_655 .
Cr2 Cr2 N4 85.8(2) 2_655 15_545
N4 Cr2 N4 171.6(5) . 15_545
Cr2 Cr2 N2 85.8(2) 2_655 .
N4 Cr2 N2 89.70(3) . .
N4 Cr2 N2 89.70(3) 15_545 .
Cr2 Cr2 N2 85.8(2) 2_655 2_655
N4 Cr2 N2 89.70(3) . 2_655
N4 Cr2 N2 89.70(3) 15_545 2_655
N2 Cr2 N2 171.7(4) . 2_655
Cr2 Cr2 Cr1 180(3) 2_655 .
N4 Cr2 Cr1 94.2(2) . .
N4 Cr2 Cr1 94.2(2) 15_545 .
N2 Cr2 Cr1 94.2(2) . .
N2 Cr2 Cr1 94.2(2) 2_655 .
N4 Cr2 Cr1 85.8(2) . 2_655
N4 Cr2 Cr1 85.8(2) 15_545 2_655
N2 Cr2 Cr1 85.8(2) . 2_655
N2 Cr2 Cr1 85.8(2) 2_655 2_655
Cr1 Cr2 Cr1 180.0 . 2_655
C15 N1 C11 118.0(10) . .
C15 N1 Cr1 123.2(8) . .
C11 N1 Cr1 118.8(8) . .
C11 N2 C11 125.2(13) . 16
C11 N2 Cr2 120.8(7) . 2_655
C11 N2 Cr2 114.0(7) 16 2_655
C11 N2 Cr2 114.0(7) . .
C11 N2 Cr2 120.8(7) 16 .
C31 N3 C35 119.6(10) . .
C31 N3 Cr1 119.0(8) . .
C35 N3 Cr1 121.1(9) . .
C31 N4 C31 127.4(13) . 2_655
C31 N4 Cr2 119.7(7) . 2_655
C31 N4 Cr2 112.8(6) 2_655 2_655
C31 N4 Cr2 112.8(6) . .
C31 N4 Cr2 119.7(7) 2_655 .
N2 C11 N1 116.2(10) . .
N2 C11 C12 124.7(11) . .
N1 C11 C12 119.0(11) . .
C13 C12 C11 121.2(12) . .
C12 C13 C14 118.4(11) . .
C12 C13 C131 124.9(19) . .
C14 C13 C131 115.7(17) . .
C12 C13 C13A 119(2) . .
C14 C13 C13A 122(2) . .
C15 C14 C13 120.2(11) . .
C14 C15 N1 123.1(11) . .
N3 C31 N4 117.3(10) . .
N3 C31 C32 120.1(11) . .
N4 C31 C32 122.3(11) . .
C33 C32 C31 120.4(12) . .
C32 C33 C34 117.8(12) . .
C32 C33 C331 120.7(12) . .
C34 C33 C331 121.5(12) . .
C35 C34 C33 120.5(12) . .
C34 C35 N3 121.6(12) . .
C13 C131 C132 131(3) . .
C13 C13A C13' 105(3) . .
C33 C331 C332 114(3) . .
I3 I2 I1 175.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N1 2.081(10) 15_545
Cr1 N1 2.081(10) .
Cr1 N3 2.125(10) .
Cr1 N3 2.125(10) 15_545
Cr1 Cr2 2.146(8) .
Cr1 Cl1 2.356(4) .
Cr1 Cr2 2.441(8) 2_655
Cr2 N4 2.025(12) .
Cr2 N4 2.025(12) 15_545
Cr2 N2 2.032(11) .
Cr2 N2 2.033(11) 2_655
Cr2 Cr1 2.441(8) 2_655
N1 C15 1.372(18) .
N1 C11 1.409(17) .
N2 C11 1.316(14) .
N2 C11 1.316(14) 16
N2 Cr2 2.032(11) 2_655
N3 C31 1.331(16) .
N3 C35 1.365(18) .
N4 C31 1.363(13) .
N4 C31 1.363(13) 2_655
N4 Cr2 2.025(12) 2_655
C11 C12 1.422(18) .
C12 C13 1.383(19) .
C13 C14 1.39(2) .
C13 C131 1.49(3) .
C13 C13A 1.51(3) .
C14 C15 1.37(2) .
C31 C32 1.420(19) .
C32 C33 1.37(2) .
C33 C34 1.39(2) .
C33 C331 1.48(2) .
C34 C35 1.36(2) .
C131 C132 1.54(4) .
C13A C13' 1.60(4) .
C331 C332 1.50(6) .
I1 I2 3.009(9) .
I2 I3 2.850(7) .
