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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/4/11/26/4112642.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_4112642
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(NCCH3)2(PF6)2.2(NCCH3)
_chemical_formula_sum            'C48 H44 Cr3 F12 N16 P2'
_chemical_formula_weight         1290.93
_chemical_name_common            Cr3(dpa)4(NCMe)2(PF6)2.2NCMe
_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                 124.6740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.0572(19)
_cell_length_b                   10.1744(7)
_cell_length_c                   22.8994(16)
_cell_measurement_reflns_used    5502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     5376.0(6)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16514
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7794
_exptl_absorpt_correction_T_min  0.7388
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0320
_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)+(0.0470P)²+5.5375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                5341
_reflns_number_total             6037
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja049055hsi20040409_043050_08.cif
_cod_data_source_block           4twoNCMe
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4112642
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 -0.080506(11) 0.93108(3) 0.253340(13) 0.02741(8) Uani 1 1 d .
Cr2 Cr -0.00552(18) 0.93307(4) 0.2504(3) 0.0228(4) Uani 0.50 1 d P
N1 N 0.12472(5) 1.02193(13) 0.34744(7) 0.0255(3) Uani 1 1 d .
N1S N 0.19454(17) 0.1134(3) 0.13187(19) 0.1120(11) Uani 1 1 d .
N2 N 0.03600(6) 1.07227(13) 0.32721(7) 0.0261(3) Uani 1 1 d .
N3 N -0.05518(6) 1.11602(13) 0.30052(7) 0.0264(3) Uani 1 1 d .
N4 N 0.09709(5) 0.74140(13) 0.29147(7) 0.0252(3) Uani 1 1 d .
N5 N 0.03680(5) 0.79254(13) 0.32641(7) 0.0253(3) Uani 1 1 d .
N6 N -0.02698(5) 0.85064(13) 0.35544(7) 0.0256(3) Uani 1 1 d .
N7 N -0.16275(7) 0.91962(15) 0.25548(8) 0.0361(3) Uani 1 1 d .
C1S C 0.20615(14) 0.1602(3) 0.09682(17) 0.0753(8) Uani 1 1 d .
C2S C 0.22077(15) 0.2206(3) 0.05196(19) 0.0862(9) Uani 1 1 d .
H1A H 0.1998 0.1781 0.0065 0.103 Uiso 1 1 calc R
H1B H 0.2616 0.2119 0.0736 0.103 Uiso 1 1 calc R
H1C H 0.2106 0.3121 0.0460 0.103 Uiso 1 1 calc R
C11 C 0.09528(7) 1.07452(15) 0.37321(9) 0.0263(3) Uani 1 1 d .
C12 C 0.12636(7) 1.11859(18) 0.44415(9) 0.0340(4) Uani 1 1 d .
H12A H 0.1065 1.1458 0.4635 0.041 Uiso 1 1 calc R
C13 C 0.18581(8) 1.1215(2) 0.48475(9) 0.0394(4) Uani 1 1 d .
H13A H 0.2062 1.1532 0.5310 0.047 Uiso 1 1 calc R
C14 C 0.21539(8) 1.0768(2) 0.45631(10) 0.0401(4) Uani 1 1 d .
H14A H 0.2556 1.0814 0.4821 0.048 Uiso 1 1 calc R
C15 C 0.18333(7) 1.02570(18) 0.38892(9) 0.0324(3) Uani 1 1 d .
H15A H 0.2030 0.9916 0.3706 0.039 Uiso 1 1 calc R
C31 C 0.00089(7) 1.15680(16) 0.33356(8) 0.0268(3) Uani 1 1 d .
C32 C 0.01730(8) 1.28072(18) 0.36709(10) 0.0362(4) Uani 1 1 d .
H32A H 0.0552 1.3098 0.3890 0.043 Uiso 1 1 calc R
C33 C -0.02248(8) 1.35883(18) 0.36764(11) 0.0398(4) Uani 1 1 d .
H33A H -0.0113 1.4398 0.3906 0.048 Uiso 1 1 calc R
C34 C -0.07953(8) 1.31597(18) 0.33360(9) 0.0356(4) Uani 1 1 d .
H34A H -0.1072 1.3674 0.3331 0.043 Uiso 1 1 calc R
C35 C -0.09364(7) 1.19612(18) 0.30094(9) 0.0320(3) Uani 1 1 d .
H35A H -0.1318 1.1678 0.2776 0.038 Uiso 1 1 calc R
C41 C 0.07363(6) 0.70325(16) 0.32718(8) 0.0274(3) Uani 1 1 d .
C42 C 0.08575(9) 0.57677(19) 0.35769(12) 0.0436(5) Uani 1 1 d .
H42A H 0.0700 0.5507 0.3823 0.052 Uiso 1 1 calc R
C43 C 0.12049(10) 0.4921(2) 0.35132(13) 0.0493(5) Uani 1 1 d .
H43A H 0.1290 0.4094 0.3722 0.059 Uiso 1 1 calc R
C44 C 0.14305(8) 0.53081(19) 0.31338(11) 0.0413(4) Uani 1 1 d .
H44A H 0.1666 0.4747 0.3082 0.050 Uiso 1 1 calc R
C45 C 0.12972(7) 0.65350(17) 0.28404(9) 0.0330(4) Uani 1 1 d .
H45A H 0.1438 0.6783 0.2574 0.040 Uiso 1 1 calc R
C61 C 0.02418(7) 0.79256(16) 0.37657(8) 0.0270(3) Uani 1 1 d .
C62 C 0.06141(8) 0.7479(2) 0.44658(10) 0.0425(4) Uani 1 1 d .
H62A H 0.0963 0.7079 0.4611 0.051 Uiso 1 1 calc R
C63 C 0.04646(9) 0.7629(2) 0.49392(10) 0.0486(5) Uani 1 1 d .
H63A H 0.0712 0.7332 0.5404 0.058 Uiso 1 1 calc R
C64 C -0.00546(8) 0.8223(2) 0.47204(9) 0.0412(4) Uani 1 1 d .
H64A H -0.0164 0.8331 0.5032 0.049 Uiso 1 1 calc R
C65 C -0.04046(7) 0.86486(18) 0.40318(9) 0.0330(4) Uani 1 1 d .
H65A H -0.0753 0.9056 0.3885 0.040 Uiso 1 1 calc R
C71 C -0.20000(7) 0.89688(18) 0.26039(9) 0.0340(4) Uani 1 1 d .
C72 C -0.24759(8) 0.8652(2) 0.26629(11) 0.0456(5) Uani 1 1 d .
H72A H -0.2681 0.7900 0.2373 0.055 Uiso 1 1 calc R
H72B H -0.2736 0.9387 0.2506 0.055 Uiso 1 1 calc R
H72C H -0.2326 0.8459 0.3149 0.055 Uiso 1 1 calc R
P1 P 0.14995(2) 0.58561(5) 0.08693(2) 0.03361(11) Uani 1 1 d .
F1 F 0.21739(5) 0.61417(17) 0.12757(8) 0.0688(4) Uani 1 1 d .
F2 F 0.08334(6) 0.55614(16) 0.04644(10) 0.0794(5) Uani 1 1 d .
F3 F 0.13742(5) 0.73947(11) 0.07478(6) 0.0488(3) Uani 1 1 d .
F4 F 0.16281(7) 0.43113(13) 0.09989(8) 0.0654(4) Uani 1 1 d .
F5 F 0.15593(7) 0.59770(14) 0.16030(7) 0.0645(4) Uani 1 1 d .
F6 F 0.14532(8) 0.57377(14) 0.01414(7) 0.0674(4) Uani 1 1 d .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N3 Cr1 N6 87.57(5) . .
N3 Cr1 N4 173.91(5) . 2
N6 Cr1 N4 90.29(5) . 2
N3 Cr1 N1 89.22(5) . 2
N6 Cr1 N1 172.73(5) . 2
N4 Cr1 N1 92.24(5) 2 2
N3 Cr1 Cr2 87.50(8) . .
N6 Cr1 Cr2 86.87(15) . .
N4 Cr1 Cr2 86.69(7) 2 .
N1 Cr1 Cr2 86.48(15) 2 .
N3 Cr1 N7 94.80(5) . .
N6 Cr1 N7 92.67(5) . .
N4 Cr1 N7 91.00(5) 2 .
N1 Cr1 N7 94.09(5) 2 .
Cr2 Cr1 N7 177.64(6) . .
N3 Cr1 Cr2 87.64(7) . 2
N6 Cr1 Cr2 87.00(13) . 2
N4 Cr1 Cr2 86.55(7) 2 2
N1 Cr1 Cr2 86.35(13) 2 2
N7 Cr1 Cr2 177.53(6) . 2
Cr2 Cr2 N2 87.4(15) 2 .
Cr2 Cr2 N5 86.4(15) 2 .
N2 Cr2 N5 88.9(2) . .
Cr2 Cr2 N5 84.5(15) 2 2
N2 Cr2 N5 171.88(16) . 2
N5 Cr2 N5 90.03(8) . 2
Cr2 Cr2 N2 83.6(15) 2 2
N2 Cr2 N2 91.14(8) . 2
N5 Cr2 N2 170.00(16) . 2
N5 Cr2 N2 88.5(2) 2 2
Cr2 Cr2 Cr1 179(2) 2 .
N2 Cr2 Cr1 93.97(15) . .
N5 Cr2 Cr1 94.15(15) . .
N5 Cr2 Cr1 94.13(15) 2 .
N2 Cr2 Cr1 95.82(16) 2 .
N2 Cr2 Cr1 86.86(13) . 2
N5 Cr2 Cr1 85.26(12) . 2
N5 Cr2 Cr1 85.03(12) 2 2
N2 Cr2 Cr1 84.76(12) 2 2
Cr1 Cr2 Cr1 178.97(8) . 2
C15 N1 C11 118.50(13) . .
C15 N1 Cr1 120.21(10) . 2
C11 N1 Cr1 121.26(10) . 2
C11 N2 C31 122.43(13) . .
C11 N2 Cr2 121.60(14) . .
C31 N2 Cr2 115.78(13) . .
C11 N2 Cr2 113.85(14) . 2
C31 N2 Cr2 123.72(14) . 2
C35 N3 C31 118.94(14) . .
C35 N3 Cr1 120.55(11) . .
C31 N3 Cr1 120.48(10) . .
C45 N4 C41 118.48(14) . .
C45 N4 Cr1 121.29(11) . 2
C41 N4 Cr1 120.21(10) . 2
C41 N5 C61 122.57(13) . .
C41 N5 Cr2 123.16(14) . .
C61 N5 Cr2 114.25(14) . .
C41 N5 Cr2 115.34(13) . 2
C61 N5 Cr2 121.98(13) . 2
C65 N6 C61 118.83(13) . .
C65 N6 Cr1 120.48(11) . .
C61 N6 Cr1 120.49(10) . .
C71 N7 Cr1 170.35(15) . .
N1S C1S C2S 179.7(4) . .
N1 C11 N2 115.34(13) . .
N1 C11 C12 119.46(14) . .
N2 C11 C12 125.08(14) . .
C13 C12 C11 120.27(15) . .
C12 C13 C14 119.66(16) . .
C15 C14 C13 117.81(16) . .
N1 C15 C14 123.91(15) . .
N3 C31 N2 114.82(14) . .
N3 C31 C32 119.30(14) . .
N2 C31 C32 125.78(15) . .
C33 C32 C31 120.41(16) . .
C32 C33 C34 119.60(17) . .
C35 C34 C33 117.95(15) . .
N3 C35 C34 123.79(16) . .
N4 C41 N5 114.91(14) . .
N4 C41 C42 119.57(14) . .
N5 C41 C42 125.42(14) . .
C43 C42 C41 120.44(17) . .
C42 C43 C44 119.53(18) . .
C45 C44 C43 118.12(16) . .
N4 C45 C44 123.78(16) . .
N6 C61 N5 114.94(13) . .
N6 C61 C62 119.78(14) . .
N5 C61 C62 125.07(14) . .
C63 C62 C61 120.17(17) . .
C62 C63 C64 119.63(17) . .
C65 C64 C63 118.25(16) . .
N6 C65 C64 123.34(16) . .
N7 C71 C72 178.9(2) . .
F2 P1 F1 179.45(10) . .
F2 P1 F3 90.82(8) . .
F1 P1 F3 89.63(8) . .
F2 P1 F5 90.77(10) . .
F1 P1 F5 89.57(8) . .
F3 P1 F5 89.36(7) . .
F2 P1 F6 90.37(10) . .
F1 P1 F6 89.29(9) . .
F3 P1 F6 90.74(7) . .
F5 P1 F6 178.85(9) . .
F2 P1 F4 89.37(9) . .
F1 P1 F4 90.19(9) . .
F3 P1 F4 179.49(7) . .
F5 P1 F4 90.17(8) . .
F6 P1 F4 89.73(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N3 2.0832(14) .
Cr1 N6 2.0967(13) .
Cr1 N4 2.1095(14) 2
Cr1 N1 2.1123(13) 2
Cr1 Cr2 2.143(3) .
Cr1 N7 2.3385(15) .
Cr1 Cr2 2.464(3) 2
Cr2 N2 2.031(4) .
Cr2 N5 2.033(4) .
Cr2 N5 2.038(4) 2
Cr2 N2 2.041(4) 2
Cr2 Cr1 2.464(3) 2
N1 C15 1.353(2) .
N1 C11 1.3680(19) .
N1 Cr1 2.1124(13) 2
N1S C1S 1.129(4) .
N2 C11 1.372(2) .
N2 C31 1.376(2) .
N2 Cr2 2.041(4) 2
N3 C35 1.357(2) .
N3 C31 1.366(2) .
N4 C45 1.358(2) .
N4 C41 1.3656(19) .
N4 Cr1 2.1096(13) 2
N5 C41 1.368(2) .
N5 C61 1.3811(19) .
N5 Cr2 2.038(4) 2
N6 C65 1.3527(19) .
N6 C61 1.361(2) .
N7 C71 1.137(2) .
C1S C2S 1.442(5) .
C11 C12 1.410(2) .
C12 C13 1.372(2) .
C13 C14 1.391(3) .
C14 C15 1.372(2) .
C31 C32 1.410(2) .
C32 C33 1.376(2) .
C33 C34 1.393(3) .
C34 C35 1.366(3) .
C41 C42 1.410(2) .
C42 C43 1.369(3) .
C43 C44 1.392(3) .
C44 C45 1.365(3) .
C61 C62 1.401(2) .
C62 C63 1.375(2) .
C63 C64 1.381(3) .
C64 C65 1.370(2) .
C71 C72 1.453(2) .
P1 F2 1.5718(14) .
P1 F1 1.5898(13) .
P1 F3 1.5938(12) .
P1 F5 1.5953(13) .
P1 F6 1.6012(13) .
P1 F4 1.6021(13) .
