#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:52:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179494 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/91/4339189.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_4339189
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            'C66 H90 Cr2 Si2'
_chemical_formula_weight         1043.56
_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                94.8270(10)
_cell_angle_beta                 114.8820(10)
_cell_angle_gamma                96.9520(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6752(4)
_cell_length_b                   12.0201(4)
_cell_length_c                   12.4185(4)
_cell_measurement_reflns_used    5869
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      1.73
_cell_volume                     1551.63(9)
_computing_cell_refinement       'SAINT (7.16b) (Bruker, 2004)'
_computing_data_collection       'Apex2 (1.0.27) (Bruker, 2004)'
_computing_data_reduction        'SAINT (7.16b) (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17987
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9587
_exptl_absorpt_correction_type   'Empirical, Twinabs (multi-scan)'
_exptl_absorpt_process_details
'TWINABS V1.05 (Sheldrick, 2003 (private commu'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         5869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0382
_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)+(0.0388P)²+0.4615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                4541
_reflns_number_total             5869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2.cif
_cod_data_source_block           rw6lf
_cod_original_cell_volume        1551.62(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339189
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
C1 C 0.82271(19) 0.85500(16) 0.34854(18) 0.0125(4) Uani 1 1 d
C2 C 0.74047(19) 0.86249(16) 0.40522(18) 0.0132(4) Uani 1 1 d
C3 C 0.6204(2) 0.79539(18) 0.36622(19) 0.0156(5) Uani 1 1 d
C4 C 0.57068(19) 0.71320(17) 0.26392(19) 0.0152(4) Uani 1 1 d
C5 C 0.6483(2) 0.70671(18) 0.20386(19) 0.0151(4) Uani 1 1 d
C6 C 0.76927(19) 0.77370(16) 0.24267(18) 0.0133(4) Uani 1 1 d
C7 C 0.78832(18) 0.94671(17) 0.51655(18) 0.0135(4) Uani 1 1 d
C8 C 0.86265(19) 0.91473(17) 0.63000(18) 0.0138(4) Uani 1 1 d
C9 C 0.9015(2) 0.99396(18) 0.73365(19) 0.0167(5) Uani 1 1 d
C10 C 0.8698(2) 1.10152(18) 0.72701(19) 0.0177(5) Uani 1 1 d
C11 C 0.8028(2) 1.13372(19) 0.61668(19) 0.0177(5) Uani 1 1 d
C12 C 0.76161(19) 1.05877(17) 0.50941(18) 0.0148(4) Uani 1 1 d
C13 C 0.8883(2) 0.79385(17) 0.64035(19) 0.0171(5) Uani 1 1 d
C14 C 0.7786(2) 0.7207(2) 0.6519(2) 0.0244(5) Uani 1 1 d
C15 C 1.0171(2) 0.7877(2) 0.7433(2) 0.0226(5) Uani 1 1 d
C16 C 0.6767(2) 1.09296(18) 0.39014(19) 0.0185(5) Uani 1 1 d
C17 C 0.5383(2) 1.0784(2) 0.3746(2) 0.0272(6) Uani 1 1 d
C18 C 0.7213(3) 1.2138(2) 0.3767(2) 0.0249(5) Uani 1 1 d
C19 C 0.83536(19) 0.74803(17) 0.16515(18) 0.0144(4) Uani 1 1 d
C20 C 0.90023(19) 0.65536(17) 0.18127(18) 0.0158(5) Uani 1 1 d
C21 C 0.9510(2) 0.62486(19) 0.1011(2) 0.0192(5) Uani 1 1 d
C22 C 0.9376(2) 0.68452(19) 0.0077(2) 0.0208(5) Uani 1 1 d
C23 C 0.8739(2) 0.77633(19) -0.00774(19) 0.0188(5) Uani 1 1 d
C24 C 0.82093(19) 0.80924(17) 0.06898(18) 0.0160(5) Uani 1 1 d
C25 C 0.9111(2) 0.58481(19) 0.2810(2) 0.0216(5) Uani 1 1 d
C26 C 0.8077(2) 0.4789(2) 0.2319(3) 0.0339(6) Uani 1 1 d
C27 C 1.0421(2) 0.5512(2) 0.3443(2) 0.0276(6) Uani 1 1 d
C28 C 0.7435(2) 0.90520(19) 0.0453(2) 0.0215(5) Uani 1 1 d
C29 C 0.7817(3) 0.9925(2) -0.0219(2) 0.0257(5) Uani 1 1 d
C30 C 0.5993(2) 0.8584(3) -0.0263(3) 0.0326(6) Uani 1 1 d
C31 C 0.3809(3) 0.5929(3) 0.3413(3) 0.0383(7) Uani 1 1 d
C32 C 0.4157(3) 0.4812(2) 0.1297(3) 0.0389(7) Uani 1 1 d
C33 C 0.2858(3) 0.6884(3) 0.1050(3) 0.0423(7) Uani 1 1 d
Si1 Si 0.41258(6) 0.61850(5) 0.20952(6) 0.02061(15) Uani 1 1 d
Cr1 Cr 1.00609(3) 0.96202(3) 0.43717(3) 0.01291(10) Uani 1 1 d
H3 H 0.573(2) 0.8087(18) 0.4116(19) 0.018(6) Uiso 1 1 d
H5 H 0.622(2) 0.6551(18) 0.1362(19) 0.015(6) Uiso 1 1 d
H9 H 0.949(2) 0.9706(18) 0.808(2) 0.017(6) Uiso 1 1 d
H10 H 0.8949(19) 1.1499(17) 0.7975(19) 0.011(5) Uiso 1 1 d
H11 H 0.7830(19) 1.2041(18) 0.6136(18) 0.012(5) Uiso 1 1 d
H13 H 0.889(2) 0.7632(18) 0.568(2) 0.017(6) Uiso 1 1 d
H14A H 0.767(2) 0.749(2) 0.724(2) 0.029(7) Uiso 1 1 d
H15B H 0.698(3) 0.719(2) 0.585(2) 0.035(7) Uiso 1 1 d
H15C H 0.793(2) 0.644(2) 0.657(2) 0.032(7) Uiso 1 1 d
H16 H 0.6808(19) 1.0418(17) 0.3293(18) 0.013(5) Uiso 1 1 d
H16A H 1.021(2) 0.8033(19) 0.822(2) 0.023(6) Uiso 1 1 d
H16B H 1.037(2) 0.714(2) 0.739(2) 0.028(6) Uiso 1 1 d
H16C H 1.087(2) 0.8418(18) 0.7393(18) 0.017(6) Uiso 1 1 d
H17A H 0.485(2) 1.099(2) 0.300(2) 0.031(7) Uiso 1 1 d
H17B H 0.506(3) 1.003(2) 0.376(2) 0.043(8) Uiso 1 1 d
H17C H 0.532(2) 1.129(2) 0.437(2) 0.039(8) Uiso 1 1 d
H18A H 0.673(2) 1.2260(19) 0.293(2) 0.026(6) Uiso 1 1 d
H18B H 0.807(2) 1.2268(19) 0.393(2) 0.023(6) Uiso 1 1 d
H18C H 0.708(2) 1.272(2) 0.432(2) 0.027(6) Uiso 1 1 d
H21 H 0.993(2) 0.5613(19) 0.1101(19) 0.019(6) Uiso 1 1 d
H22 H 0.9707(19) 0.6615(17) -0.0469(19) 0.013(5) Uiso 1 1 d
H23 H 0.8666(19) 0.8172(17) -0.0723(19) 0.012(5) Uiso 1 1 d
H25 H 0.900(2) 0.6297(19) 0.340(2) 0.022(6) Uiso 1 1 d
H26A H 0.817(3) 0.432(2) 0.171(3) 0.047(9) Uiso 1 1 d
H26B H 0.812(2) 0.434(2) 0.296(2) 0.041(8) Uiso 1 1 d
H26C H 0.720(3) 0.495(2) 0.198(2) 0.039(7) Uiso 1 1 d
H27A H 1.048(2) 0.511(2) 0.412(2) 0.027(6) Uiso 1 1 d
H27A H 1.112(3) 0.615(2) 0.379(2) 0.038(7) Uiso 1 1 d
H27B H 1.061(2) 0.500(2) 0.288(2) 0.037(7) Uiso 1 1 d
H28 H 0.756(2) 0.9429(19) 0.122(2) 0.024(6) Uiso 1 1 d
H29A H 0.875(3) 1.017(2) 0.013(2) 0.030(7) Uiso 1 1 d
H29B H 0.757(2) 0.9641(19) -0.104(2) 0.022(6) Uiso 1 1 d
H29C H 0.742(2) 1.057(2) -0.020(2) 0.034(7) Uiso 1 1 d
H30A H 0.584(3) 0.808(2) -0.103(3) 0.050(8) Uiso 1 1 d
H30C H 0.553(2) 0.922(2) -0.043(2) 0.034(7) Uiso 1 1 d
H31A H 0.449(3) 0.559(3) 0.396(3) 0.073(11) Uiso 1 1 d
H31B H 0.377(3) 0.662(2) 0.384(2) 0.044(8) Uiso 1 1 d
H31C H 0.300(3) 0.549(2) 0.316(3) 0.053(9) Uiso 1 1 d
H32A H 0.329(3) 0.431(2) 0.099(3) 0.055(9) Uiso 1 1 d
H32B H 0.474(3) 0.440(3) 0.185(3) 0.058(10) Uiso 1 1 d
H32C H 0.433(3) 0.492(3) 0.061(3) 0.057(9) Uiso 1 1 d
H33A H 0.306(3) 0.707(2) 0.041(3) 0.044(8) Uiso 1 1 d
H33B H 0.282(3) 0.754(3) 0.151(3) 0.060(10) Uiso 1 1 d
H33C H 0.206(3) 0.642(3) 0.074(3) 0.069(10) Uiso 1 1 d
H39B H 0.570(3) 0.812(2) 0.017(2) 0.043(8) 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'
Si Si 0.0817 0.0704 '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
C2 C1 C6 113.43(17) . .
C2 C1 Cr1 115.73(14) . .
C6 C1 Cr1 130.81(14) . .
C3 C2 C1 124.79(19) . .
C3 C2 C7 118.09(18) . .
C1 C2 C7 117.10(17) . .
C2 C3 C4 121.1(2) . .
C3 C4 C5 115.19(19) . .
C3 C4 Si1 123.12(16) . .
C5 C4 Si1 121.69(16) . .
C4 C5 C6 123.97(19) . .
C5 C6 C1 121.42(18) . .
C5 C6 C19 113.81(17) . .
C1 C6 C19 124.75(17) . .
C12 C7 C8 120.10(18) . .
C12 C7 C2 120.23(18) . .
C8 C7 C2 119.66(18) . .
C12 C7 Cr1 82.40(12) . 2_776
C8 C7 Cr1 77.37(11) . 2_776
C2 C7 Cr1 109.74(12) . 2_776
C9 C8 C7 118.45(19) . .
C9 C8 C13 120.26(19) . .
C7 C8 C13 121.01(18) . .
C9 C8 Cr1 89.84(12) . 2_776
C7 C8 Cr1 67.97(11) . 2_776
C13 C8 Cr1 116.84(13) . 2_776
C10 C9 C8 121.3(2) . .
C11 C10 C9 119.9(2) . .
C10 C11 C12 121.6(2) . .
C11 C12 C7 118.43(19) . .
C11 C12 C16 120.19(19) . .
C7 C12 C16 120.96(18) . .
C8 C13 C15 112.87(18) . .
C8 C13 C14 110.05(18) . .
C15 C13 C14 111.00(19) . .
C12 C16 C18 113.25(19) . .
C12 C16 C17 109.40(19) . .
C18 C16 C17 110.5(2) . .
C20 C19 C24 120.43(19) . .
C20 C19 C6 119.12(18) . .
C24 C19 C6 120.12(18) . .
C21 C20 C19 118.9(2) . .
C21 C20 C25 119.90(19) . .
C19 C20 C25 121.10(18) . .
C22 C21 C20 120.8(2) . .
C21 C22 C23 120.2(2) . .
C22 C23 C24 121.1(2) . .
C23 C24 C19 118.55(19) . .
C23 C24 C28 120.25(19) . .
C19 C24 C28 121.13(18) . .
C27 C25 C26 109.6(2) . .
C27 C25 C20 113.65(19) . .
C26 C25 C20 110.5(2) . .
C24 C28 C29 114.03(19) . .
C24 C28 C30 110.8(2) . .
C29 C28 C30 108.3(2) . .
C33 Si1 C4 109.10(12) . .
C33 Si1 C31 109.98(16) . .
C4 Si1 C31 108.69(12) . .
C33 Si1 C32 109.59(16) . .
C4 Si1 C32 109.65(11) . .
C31 Si1 C32 109.81(15) . .
Cr1 Cr1 C1 101.65(6) 2_776 .
Cr1 Cr1 C7 95.73(5) 2_776 2_776
C1 Cr1 C7 162.58(7) . 2_776
Cr1 Cr1 C8 109.81(5) 2_776 2_776
C1 Cr1 C8 134.23(7) . 2_776
C7 Cr1 C8 34.66(7) 2_776 2_776
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.416(3) .
C1 C6 1.421(3) .
C1 Cr1 2.136(2) .
C2 C3 1.393(3) .
C2 C7 1.492(3) .
C3 C4 1.399(3) .
C4 C5 1.400(3) .
C4 Si1 1.863(2) .
C5 C6 1.401(3) .
C6 C19 1.500(3) .
C7 C12 1.420(3) .
C7 C8 1.424(3) .
C7 Cr1 2.3218(19) 2_776
C8 C9 1.403(3) .
C8 C13 1.524(3) .
C8 Cr1 2.4439(19) 2_776
C9 C10 1.387(3) .
C10 C11 1.378(3) .
C11 C12 1.404(3) .
C12 C16 1.520(3) .
C13 C15 1.525(3) .
C13 C14 1.528(3) .
C16 C18 1.530(3) .
C16 C17 1.530(3) .
C19 C20 1.403(3) .
C19 C24 1.416(3) .
C20 C21 1.401(3) .
C20 C25 1.530(3) .
C21 C22 1.378(3) .
C22 C23 1.386(3) .
C23 C24 1.392(3) .
C24 C28 1.523(3) .
C25 C27 1.520(3) .
C25 C26 1.526(3) .
C28 C29 1.531(3) .
C28 C30 1.539(3) .
C31 Si1 1.865(3) .
C32 Si1 1.865(3) .
C33 Si1 1.857(3) .
Cr1 Cr1 1.8077(7) 2_776
Cr1 C7 2.3218(19) 2_776
Cr1 C8 2.4439(19) 2_776
