#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:52:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179494 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/91/4339190.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_4339190
loop_
_publ_author_name
'Wolf, Robert'
'Ni, Chengbao'
'Nguyen, Tailuan'
'Brynda, Marcin'
'Long, Gary J.'
'Sutton, Andrew D.'
'Fischer, Roland C.'
'Fettinger, J. C.'
'Hellman, Matthew'
'Pu, Lihung'
'Power, Philip P.'
_publ_section_title
;
 Substituent effects in formally quintuple-bonded ArCrCrAr compounds (Ar =
 terphenyl) and related species.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11277
_journal_page_last               11290
_journal_paper_doi               10.1021/ic702112e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C76 H94 Cr2 O2'
_chemical_formula_weight         1143.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.655(2)
_cell_angle_beta                 92.661(2)
_cell_angle_gamma                105.614(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2466(8)
_cell_length_b                   11.1972(9)
_cell_length_c                   15.2070(12)
_cell_measurement_reflns_used    7593
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.4962
_cell_measurement_theta_min      0.970897
_cell_volume                     1564.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART software'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'WinGX v1.64.59 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'ω and φ'
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23869
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9768
_exptl_absorpt_correction_T_min  0.8745
_exptl_absorpt_correction_type   'Empirical, Twinabs (multi-scan)'
_exptl_absorpt_process_details   'TWINABS V1.05 (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    'located on diff map and refined freely'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0610P)²+0.7495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                6876
_reflns_number_total             9062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            3.cif
_cod_data_source_block           rw31fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339190
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Cr1 Cr -0.06966(2) -0.00214(2) 0.034799(18) 0.01199(7) Uani 1 1 d
O1 O 0.29199(11) 0.06635(12) 0.41029(8) 0.0173(2) Uani 1 1 d
C1 C 0.02673(15) 0.00856(14) 0.16561(11) 0.0113(3) Uani 1 1 d
C2 C 0.16939(15) 0.02244(14) 0.17038(11) 0.0112(3) Uani 1 1 d
C3 C 0.25549(15) 0.04122(15) 0.25055(11) 0.0130(3) Uani 1 1 d
C4 C 0.20092(16) 0.04491(15) 0.33309(11) 0.0135(3) Uani 1 1 d
C5 C 0.06161(16) 0.02728(15) 0.33243(11) 0.0132(3) Uani 1 1 d
C6 C -0.02363(15) 0.01056(14) 0.25123(11) 0.0111(3) Uani 1 1 d
C7 C 0.23109(14) 0.01553(15) 0.08230(11) 0.0111(3) Uani 1 1 d
C8 C 0.22033(15) -0.11050(15) 0.01227(11) 0.0128(3) Uani 1 1 d
C9 C 0.28496(16) -0.11411(17) -0.06764(12) 0.0166(3) Uani 1 1 d
C10 C 0.35637(16) 0.00186(17) -0.08018(12) 0.0169(3) Uani 1 1 d
C11 C 0.36090(16) 0.12457(17) -0.01437(12) 0.0165(3) Uani 1 1 d
C12 C 0.29872(15) 0.13425(15) 0.06712(11) 0.0133(3) Uani 1 1 d
C13 C -0.17157(15) -0.00646(15) 0.26482(11) 0.0121(3) Uani 1 1 d
C14 C -0.21289(16) 0.10636(16) 0.31187(11) 0.0146(3) Uani 1 1 d
C15 C -0.34681(16) 0.08828(17) 0.33194(12) 0.0166(3) Uani 1 1 d
C16 C -0.43842(16) -0.03784(17) 0.30728(12) 0.0171(3) Uani 1 1 d
C17 C -0.39798(16) -0.14878(17) 0.26101(12) 0.0160(3) Uani 1 1 d
C18 C -0.26493(16) -0.13541(16) 0.23948(11) 0.0142(3) Uani 1 1 d
C19 C 0.15497(16) -0.23988(16) 0.02793(12) 0.0156(3) Uani 1 1 d
C20 C -0.11357(17) 0.24692(16) 0.34453(13) 0.0183(3) Uani 1 1 d
C21 C 0.26449(19) -0.27760(19) 0.07554(14) 0.0228(4) Uani 1 1 d
C22 C 0.46109(19) 0.31968(19) 0.20174(14) 0.0228(4) Uani 1 1 d
C23 C -0.22172(17) -0.25970(16) 0.19302(14) 0.0206(3) Uani 1 1 d
C24 C 0.31853(17) 0.27054(16) 0.14219(12) 0.0165(3) Uani 1 1 d
C25 C 0.30163(19) 0.37346(18) 0.10079(14) 0.0214(4) Uani 1 1 d
C26 C -0.05091(19) 0.29589(19) 0.44922(14) 0.0239(4) Uani 1 1 d
C27 C -0.3411(2) -0.38176(18) 0.13406(14) 0.0251(4) Uani 1 1 d
C28 C -0.1786(2) 0.34941(18) 0.33086(14) 0.0233(4) Uani 1 1 d
C29 C 0.07978(19) -0.35445(18) -0.06389(14) 0.0222(4) Uani 1 1 d
C30 C -0.1514(2) -0.2964(2) 0.2672(2) 0.0403(6) Uani 1 1 d
C32 C 0.29773(19) 0.52420(18) 0.39592(14) 0.0243(4) Uani 1 1 d
C31 C 0.2362(2) 0.0676(2) 0.49496(13) 0.0275(4) Uani 1 1 d
C33 C 0.38273(19) 0.65526(19) 0.43989(14) 0.0248(4) Uani 1 1 d
C34 C 0.36071(19) 0.75716(18) 0.41455(14) 0.0243(4) Uani 1 1 d
C35 C 0.25470(19) 0.73015(19) 0.34380(14) 0.0246(4) Uani 1 1 d
C36 C 0.17065(19) 0.60062(19) 0.29872(14) 0.0258(4) Uani 1 1 d
C37 C 0.19223(19) 0.49905(19) 0.32536(14) 0.0255(4) Uani 1 1 d
C38 C 0.3197(3) 0.4138(2) 0.42408(18) 0.0335(5) Uani 1 1 d
H20 H -0.042(2) 0.2441(19) 0.3071(14) 0.015(5) Uiso 1 1 d
H37 H 0.134(2) 0.406(2) 0.2951(17) 0.034(6) Uiso 1 1 d
H23 H 0.376(2) 0.396(2) 0.0687(15) 0.021(5) Uiso 1 1 d
H8 H 0.4012(19) 0.0025(19) -0.1324(14) 0.014(5) Uiso 1 1 d
H14 H 0.090(2) -0.2255(19) 0.0694(14) 0.014(5) Uiso 1 1 d
H2 H -0.527(2) -0.048(2) 0.3224(15) 0.022(5) Uiso 1 1 d
H10 H 0.277(2) -0.198(2) -0.1128(15) 0.020(5) Uiso 1 1 d
H3 H -0.376(2) 0.161(2) 0.3625(14) 0.018(5) Uiso 1 1 d
H1 H -0.460(2) -0.236(2) 0.2437(15) 0.024(5) Uiso 1 1 d
H18 H 0.460(2) 0.674(2) 0.4876(17) 0.029(6) Uiso 1 1 d
H25 H 0.252(2) 0.262(2) 0.1813(15) 0.018(5) Uiso 1 1 d
H22 H 0.299(2) 0.452(2) 0.1491(16) 0.025(5) Uiso 1 1 d
H17 H 0.537(2) 0.330(2) 0.1622(16) 0.025(5) Uiso 1 1 d
H21 H 0.098(2) 0.579(2) 0.2479(16) 0.026(6) Uiso 1 1 d
H20 H 0.237(2) 0.797(2) 0.3195(15) 0.024(5) Uiso 1 1 d
H24 H 0.215(2) 0.342(2) 0.0584(16) 0.024(5) Uiso 1 1 d
H9 H 0.407(2) 0.206(2) -0.0254(15) 0.023(5) Uiso 1 1 d
H16 H 0.474(2) 0.403(2) 0.2506(16) 0.023(5) Uiso 1 1 d
H13 H 0.309(2) -0.208(2) 0.1349(17) 0.029(6) Uiso 1 1 d
H7 H -0.305(2) -0.453(2) 0.0958(17) 0.035(6) Uiso 1 1 d
H11 H 0.222(2) -0.360(2) 0.0866(16) 0.026(6) Uiso 1 1 d
H4 H -0.161(2) -0.240(2) 0.1509(16) 0.027(6) Uiso 1 1 d
H15 H 0.471(2) 0.261(2) 0.2304(16) 0.026(6) Uiso 1 1 d
H5 H -0.402(2) -0.417(2) 0.1755(17) 0.032(6) Uiso 1 1 d
H19 H 0.416(2) 0.845(2) 0.4474(16) 0.028(6) Uiso 1 1 d
H6 H -0.404(2) -0.363(2) 0.0884(18) 0.039(7) Uiso 1 1 d
H12 H 0.334(2) -0.293(2) 0.0321(18) 0.036(6) Uiso 1 1 d
H26 H 0.313(2) 0.087(2) 0.5426(17) 0.031(6) Uiso 1 1 d
H36 H -0.245(2) 0.364(2) 0.3741(17) 0.029(6) Uiso 1 1 d
H28 H 0.191(2) 0.136(2) 0.5157(15) 0.022(5) Uiso 1 1 d
H35 H -0.109(2) 0.436(2) 0.3433(16) 0.032(6) Uiso 1 1 d
H34 H -0.122(2) 0.302(2) 0.4883(16) 0.028(6) Uiso 1 1 d
H33 H 0.014(2) 0.381(2) 0.4682(17) 0.032(6) Uiso 1 1 d
H32 H -0.004(2) 0.237(2) 0.4624(16) 0.032(6) Uiso 1 1 d
H29 H -0.225(3) -0.327(3) 0.3062(19) 0.049(8) Uiso 1 1 d
H31 H -0.067(3) -0.229(3) 0.304(2) 0.056(8) Uiso 1 1 d
H39 H 0.412(3) 0.404(3) 0.415(2) 0.051(8) Uiso 1 1 d
H76 H -0.227(3) 0.322(3) 0.2650(19) 0.045(7) Uiso 1 1 d
H30 H -0.128(3) -0.378(3) 0.232(2) 0.062(9) Uiso 1 1 d
H38 H 0.310(3) 0.430(3) 0.490(2) 0.049(8) Uiso 1 1 d
H27 H 0.168(3) -0.022(3) 0.4817(18) 0.040(7) Uiso 1 1 d
H40 H 0.252(3) 0.332(3) 0.390(2) 0.068(10) Uiso 1 1 d
H42 H 0.016(2) -0.331(2) -0.1002(17) 0.032(6) Uiso 1 1 d
H41 H 0.144(2) -0.382(2) -0.1064(18) 0.038(7) Uiso 1 1 d
H43 H 0.026(3) -0.428(3) -0.0469(18) 0.040(7) Uiso 1 1 d
H46 H 0.351(2) 0.0528(19) 0.2502(14) 0.015(5) Uiso 1 1 d
H45 H 0.020(2) 0.0238(19) 0.3851(15) 0.017(5) Uiso 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'
O O 0.0106 0.0060 '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
Cr1 Cr1 C1 102.25(4) 2 .
Cr1 Cr1 C7 95.37(4) 2 2
C1 Cr1 C7 162.38(6) . 2
Cr1 Cr1 C8 108.53(4) 2 2
C1 Cr1 C8 135.31(5) . 2
C7 Cr1 C8 34.61(5) 2 2
C4 O1 C31 116.58(13) . .
C6 C1 C2 113.31(13) . .
C6 C1 Cr1 131.81(11) . .
C2 C1 Cr1 114.81(11) . .
C3 C2 C1 125.01(14) . .
C3 C2 C7 117.58(13) . .
C1 C2 C7 117.41(13) . .
C4 C3 C2 119.13(14) . .
O1 C4 C5 124.92(15) . .
O1 C4 C3 116.23(13) . .
C5 C4 C3 118.86(14) . .
C4 C5 C6 121.28(15) . .
C5 C6 C1 122.35(13) . .
C5 C6 C13 113.27(13) . .
C1 C6 C13 124.37(13) . .
C12 C7 C8 119.67(14) . .
C12 C7 C2 120.35(13) . .
C8 C7 C2 119.97(13) . .
C12 C7 Cr1 81.09(9) . 2
C8 C7 Cr1 78.31(9) . 2
C2 C7 Cr1 109.92(9) . 2
C9 C8 C7 118.77(14) . .
C9 C8 C19 119.56(14) . .
C7 C8 C19 121.28(14) . .
C9 C8 Cr1 90.07(10) . 2
C7 C8 Cr1 67.08(8) . 2
C19 C8 Cr1 118.56(10) . 2
C10 C9 C8 121.40(15) . .
C9 C10 C11 119.81(15) . .
C10 C11 C12 121.23(15) . .
C11 C12 C7 118.96(14) . .
C11 C12 C24 119.47(14) . .
C7 C12 C24 121.21(14) . .
C14 C13 C18 120.02(14) . .
C14 C13 C6 119.68(13) . .
C18 C13 C6 119.97(13) . .
C15 C14 C13 119.07(14) . .
C15 C14 C20 119.18(14) . .
C13 C14 C20 121.71(13) . .
C16 C15 C14 121.05(15) . .
C15 C16 C17 119.95(15) . .
C16 C17 C18 120.97(15) . .
C17 C18 C13 118.94(14) . .
C17 C18 C23 119.58(14) . .
C13 C18 C23 121.43(13) . .
C8 C19 C21 109.77(13) . .
C8 C19 C29 112.56(14) . .
C21 C19 C29 110.45(14) . .
C14 C20 C28 113.53(14) . .
C14 C20 C26 111.48(15) . .
C28 C20 C26 108.46(14) . .
C18 C23 C27 113.52(14) . .
C18 C23 C30 111.09(16) . .
C27 C23 C30 107.67(16) . .
C12 C24 C25 112.99(14) . .
C12 C24 C22 109.42(13) . .
C25 C24 C22 109.90(14) . .
C37 C32 C33 117.94(18) . .
C37 C32 C38 120.90(18) . .
C33 C32 C38 121.16(19) . .
C34 C33 C32 120.92(18) . .
C35 C34 C33 120.34(18) . .
C36 C35 C34 119.47(18) . .
C35 C36 C37 119.89(18) . .
C32 C37 C36 121.43(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 Cr1 1.8160(5) 2
Cr1 C1 2.1308(15) .
Cr1 C7 2.3114(14) 2
Cr1 C8 2.4576(15) 2
O1 C4 1.3765(18) .
O1 C31 1.430(2) .
C1 C6 1.418(2) .
C1 C2 1.424(2) .
C2 C3 1.392(2) .
C2 C7 1.495(2) .
C3 C4 1.390(2) .
C4 C5 1.386(2) .
C5 C6 1.407(2) .
C6 C13 1.509(2) .
C7 C12 1.423(2) .
C7 C8 1.426(2) .
C7 Cr1 2.3114(14) 2
C8 C9 1.405(2) .
C8 C19 1.526(2) .
C8 Cr1 2.4576(15) 2
C9 C10 1.388(2) .
C10 C11 1.388(2) .
C11 C12 1.405(2) .
C12 C24 1.521(2) .
C13 C14 1.412(2) .
C13 C18 1.413(2) .
C14 C15 1.396(2) .
C14 C20 1.525(2) .
C15 C16 1.383(2) .
C16 C17 1.388(2) .
C17 C18 1.397(2) .
C18 C23 1.527(2) .
C19 C21 1.532(2) .
C19 C29 1.534(2) .
C20 C28 1.538(2) .
C20 C26 1.541(3) .
C22 C24 1.538(2) .
C23 C27 1.530(2) .
C23 C30 1.535(3) .
C24 C25 1.530(2) .
C32 C37 1.387(3) .
C32 C33 1.399(3) .
C32 C38 1.503(3) .
C33 C34 1.388(3) .
C34 C35 1.387(3) .
C35 C36 1.385(3) .
C36 C37 1.394(3) .
