#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:52:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179494 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/91/4339195.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_4339195
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            'C84 H104 Cr2 F8 O2'
_chemical_formula_weight         1401.67
_chemical_melting_point          212
_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                101.9990(10)
_cell_angle_beta                 98.7800(10)
_cell_angle_gamma                93.1030(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8443(5)
_cell_length_b                   13.8545(7)
_cell_length_c                   14.2731(8)
_cell_measurement_reflns_used    2956
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      1.64
_cell_volume                     1874.39(17)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART SOFTWARE'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'SHELXTL 97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.572
_diffrn_measured_fraction_theta_max 0.572
_diffrn_measurement_device_type  'Bruker Smart1000'
_diffrn_measurement_method       'Omega Scans'
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14994
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9552
_exptl_absorpt_correction_T_min  0.9227
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         6037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                4701
_reflns_number_total             6037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            5.cif
_cod_data_source_block           rw43fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339195
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
_atom_site_refinement_flags
Cr1 Cr 0.56976(3) 0.56254(2) 0.60105(2) 0.01580(10) Uani 1 1 d .
F1 F 0.38594(13) 0.50667(10) 0.52904(9) 0.0226(2) Uani 1 1 d .
F2 F 0.28328(16) 0.78775(13) 1.01054(10) 0.0339(3) Uani 1 1 d .
F3 F 0.17450(16) 0.85559(12) 0.90381(11) 0.0342(3) Uani 1 1 d .
F4 F 0.10483(17) 0.70980(14) 0.91399(14) 0.0486(5) Uani 1 1 d .
O1 O 0.77786(15) 0.59448(12) 0.64915(11) 0.0233(3) Uani 1 1 d .
C1 C 0.48518(18) 0.64070(13) 0.71928(12) 0.0149(3) Uani 1 1 d .
C2 C 0.45024(18) 0.73986(14) 0.72741(13) 0.0151(3) Uani 1 1 d .
C3 C 0.35939(19) 0.78037(14) 0.78818(13) 0.0170(3) Uani 1 1 d .
H3 H 0.327(3) 0.848(2) 0.788(2) 0.019(6) Uiso 1 1 d .
C4 C 0.30806(19) 0.72514(14) 0.84791(13) 0.0173(3) Uani 1 1 d .
C5 C 0.34658(18) 0.62999(14) 0.84717(13) 0.0167(3) Uani 1 1 d .
H5 H 0.319(3) 0.594(2) 0.892(2) 0.030(7) Uiso 1 1 d .
C6 C 0.43183(18) 0.58765(13) 0.78299(13) 0.0148(3) Uani 1 1 d .
C7 C 0.46972(18) 0.48469(14) 0.78805(13) 0.0149(3) Uani 1 1 d .
C8 C 0.37498(19) 0.40149(14) 0.74611(14) 0.0179(3) Uani 1 1 d .
C12 C 0.59917(19) 0.47278(15) 0.84200(14) 0.0184(4) Uani 1 1 d .
C9 C 0.4095(2) 0.30765(15) 0.75974(15) 0.0227(4) Uani 1 1 d .
H9 H 0.344(3) 0.251(2) 0.731(2) 0.024(7) Uiso 1 1 d .
C10 C 0.5351(2) 0.29600(16) 0.81216(16) 0.0242(4) Uani 1 1 d .
H10 H 0.566(3) 0.234(2) 0.824(2) 0.021(6) Uiso 1 1 d .
C11 C 0.6293(2) 0.37770(17) 0.85226(15) 0.0224(4) Uani 1 1 d .
H11 H 0.710(4) 0.367(3) 0.892(3) 0.040(9) Uiso 1 1 d .
C13 C 0.51631(19) 0.80784(14) 0.67404(14) 0.0182(3) Uani 1 1 d .
C14 C 0.4705(2) 0.80205(16) 0.57407(15) 0.0216(4) Uani 1 1 d .
C15 C 0.5368(3) 0.8648(2) 0.52664(19) 0.0350(6) Uani 1 1 d .
H15 H 0.508(3) 0.857(2) 0.461(2) 0.027(7) Uiso 1 1 d .
C16 C 0.6460(3) 0.9326(2) 0.5769(2) 0.0449(7) Uani 1 1 d .
H16 H 0.693(4) 0.981(3) 0.544(3) 0.049(10) Uiso 1 1 d .
C17 C 0.6884(3) 0.9408(2) 0.6759(2) 0.0368(6) Uani 1 1 d .
H17 H 0.755(5) 0.985(4) 0.710(3) 0.063(12) Uiso 1 1 d .
C18 C 0.6256(2) 0.87879(16) 0.72586(16) 0.0231(4) Uani 1 1 d .
C19 C 0.2189(2) 0.76942(16) 0.91839(15) 0.0211(4) Uani 1 1 d .
C20 C 0.2336(2) 0.40976(15) 0.69051(15) 0.0224(4) Uani 1 1 d .
H20 H 0.241(3) 0.475(2) 0.675(2) 0.030(7) Uiso 1 1 d .
C21 C 0.1966(3) 0.32924(18) 0.59659(17) 0.0301(5) Uani 1 1 d .
H21A H 0.104(4) 0.340(3) 0.556(3) 0.043(9) Uiso 1 1 d .
H21C H 0.273(3) 0.333(2) 0.548(2) 0.024(7) Uiso 1 1 d .
H21B H 0.183(4) 0.270(3) 0.618(3) 0.050(10) Uiso 1 1 d .
C22 C 0.1241(2) 0.4048(2) 0.75556(19) 0.0296(5) Uani 1 1 d .
H22C H 0.035(4) 0.406(3) 0.718(2) 0.033(8) Uiso 1 1 d .
H22B H 0.140(4) 0.467(3) 0.811(3) 0.038(8) Uiso 1 1 d .
H22A H 0.125(4) 0.362(3) 0.788(3) 0.056(11) Uiso 1 1 d .
C23 C 0.6989(2) 0.56179(17) 0.89390(15) 0.0228(4) Uani 1 1 d .
H23 H 0.695(3) 0.612(3) 0.854(3) 0.038(8) Uiso 1 1 d .
C24 C 0.8498(2) 0.5378(3) 0.9065(3) 0.0439(7) Uani 1 1 d .
H24B H 0.872(4) 0.503(3) 0.960(3) 0.042(9) Uiso 1 1 d .
H24C H 0.911(4) 0.602(3) 0.924(3) 0.044(9) Uiso 1 1 d .
H24A H 0.877(4) 0.510(3) 0.846(3) 0.048(10) Uiso 1 1 d .
C25 C 0.6604(3) 0.6071(2) 0.99315(18) 0.0352(5) Uani 1 1 d .
H25B H 0.726(3) 0.661(3) 1.025(2) 0.028(7) Uiso 1 1 d .
H25C H 0.563(4) 0.626(3) 0.984(3) 0.046(9) Uiso 1 1 d .
H25A H 0.671(4) 0.556(3) 1.032(3) 0.049(10) Uiso 1 1 d .
C26 C 0.3433(2) 0.73563(15) 0.51943(14) 0.0209(4) Uani 1 1 d .
H26 H 0.326(3) 0.680(2) 0.553(2) 0.020(6) Uiso 1 1 d .
C27 C 0.3556(3) 0.6890(2) 0.41453(18) 0.0359(5) Uani 1 1 d .
H27C H 0.271(5) 0.633(4) 0.390(4) 0.084(15) Uiso 1 1 d .
H27B H 0.316(6) 0.734(5) 0.364(4) 0.089(16) Uiso 1 1 d .
H27A H 0.446(5) 0.656(4) 0.422(4) 0.089(17) Uiso 1 1 d .
C28 C 0.2167(2) 0.79531(19) 0.5222(2) 0.0318(5) Uani 1 1 d .
H28C H 0.140(3) 0.749(3) 0.487(2) 0.028(7) Uiso 1 1 d .
H28B H 0.239(3) 0.841(3) 0.489(2) 0.037(8) Uiso 1 1 d .
H28A H 0.198(3) 0.822(3) 0.592(3) 0.037(8) Uiso 1 1 d .
C29 C 0.6749(2) 0.89156(17) 0.83515(16) 0.0256(4) Uani 1 1 d .
H29 H 0.650(3) 0.832(2) 0.855(2) 0.021(6) Uiso 1 1 d .
C30 C 0.8316(3) 0.9166(2) 0.86549(19) 0.0330(5) Uani 1 1 d .
H30C H 0.886(4) 0.871(3) 0.832(3) 0.051(10) Uiso 1 1 d .
H30B H 0.863(4) 0.908(3) 0.940(3) 0.051(10) Uiso 1 1 d .
H30A H 0.855(4) 0.992(3) 0.854(3) 0.044(9) Uiso 1 1 d .
C31 C 0.6027(3) 0.9726(2) 0.8923(2) 0.0440(7) Uani 1 1 d .
H31C H 0.627(4) 1.043(3) 0.880(3) 0.044(9) Uiso 1 1 d .
H31B H 0.493(4) 0.959(3) 0.881(3) 0.045(9) Uiso 1 1 d .
H31A H 0.649(5) 0.981(4) 0.966(4) 0.065(12) Uiso 1 1 d .
C32 C 0.8377(2) 0.68781(19) 0.71440(17) 0.0289(4) Uani 1 1 d .
H32B H 0.868(4) 0.677(3) 0.792(3) 0.041(9) Uiso 1 1 d .
H32A H 0.765(3) 0.734(3) 0.711(2) 0.029(7) Uiso 1 1 d .
C33 C 0.9595(2) 0.71866(17) 0.67003(17) 0.0251(4) Uani 1 1 d .
H33B H 0.944(3) 0.745(3) 0.612(2) 0.032(8) Uiso 1 1 d .
H33A H 1.028(3) 0.764(3) 0.714(2) 0.032(8) Uiso 1 1 d .
C34 C 1.0142(2) 0.61992(19) 0.63627(19) 0.0286(4) Uani 1 1 d .
H34B H 1.069(4) 0.623(3) 0.588(3) 0.050(10) Uiso 1 1 d .
H34A H 1.069(4) 0.599(3) 0.686(3) 0.053(11) Uiso 1 1 d .
C35 C 0.8859(2) 0.54777(17) 0.60061(17) 0.0257(4) Uani 1 1 d .
H35B H 0.897(4) 0.484(3) 0.617(3) 0.050(10) Uiso 1 1 d .
H35A H 0.843(3) 0.541(3) 0.530(3) 0.036(8) Uiso 1 1 d .
C36 C 0.0285(3) 0.1409(2) 0.7784(2) 0.0427(7) Uani 1 1 d .
C37 C 0.0297(3) 0.0988(2) 0.6826(2) 0.0403(6) Uani 1 1 d .
H37 H -0.065(4) 0.106(3) 0.640(3) 0.054(11) Uiso 1 1 d .
C38 C 0.1422(4) 0.0492(2) 0.6553(3) 0.0487(7) Uani 1 1 d .
H38 H 0.124(6) 0.020(5) 0.587(5) 0.086(16) Uiso 1 1 d .
C39 C 0.2521(4) 0.0406(2) 0.7234(4) 0.0610(11) Uani 1 1 d .
H39 H 0.3283 0.0066 0.7049 0.073 Uiso 1 1 calc R
C40 C 0.2500(5) 0.0825(3) 0.8198(4) 0.0697(13) Uani 1 1 d .
H40 H 0.3255 0.0775 0.8682 0.084 Uiso 1 1 calc R
C41 C 0.1398(5) 0.1310(3) 0.8461(3) 0.0599(10) Uani 1 1 d .
H41 H 0.1399 0.1587 0.9128 0.072 Uiso 1 1 calc R
C42 C -0.0918(5) 0.1963(3) 0.8061(4) 0.0768(16) Uani 1 1 d .
H42A H -0.0767 0.2215 0.8767 0.115 Uiso 1 1 calc R
H42B H -0.1766 0.1516 0.7862 0.115 Uiso 1 1 calc R
H42C H -0.1003 0.2519 0.7736 0.115 Uiso 1 1 calc R
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'
F F 0.0171 0.0103 '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
F1 Cr1 F1 77.89(6) . 2_666
F1 Cr1 O1 165.34(6) . .
F1 Cr1 O1 88.17(6) 2_666 .
F1 Cr1 C1 92.15(6) . .
F1 Cr1 C1 168.02(6) 2_666 .
O1 Cr1 C1 102.21(7) . .
Cr1 F1 Cr1 102.11(6) . 2_666
C32 O1 C35 108.74(16) . .
C32 O1 Cr1 123.10(13) . .
C35 O1 Cr1 125.03(14) . .
C2 C1 C6 115.92(16) . .
C2 C1 Cr1 123.23(12) . .
C6 C1 Cr1 119.38(13) . .
C3 C2 C1 122.13(15) . .
C3 C2 C13 117.06(16) . .
C1 C2 C13 120.74(16) . .
C4 C3 C2 119.70(17) . .
C3 C4 C5 120.16(17) . .
C3 C4 C19 120.59(17) . .
C5 C4 C19 119.12(16) . .
C4 C5 C6 120.15(16) . .
C5 C6 C1 121.71(16) . .
C5 C6 C7 116.52(15) . .
C1 C6 C7 121.71(16) . .
C8 C7 C12 119.91(16) . .
C8 C7 C6 120.86(15) . .
C12 C7 C6 119.07(17) . .
C9 C8 C7 119.15(17) . .
C9 C8 C20 118.38(17) . .
C7 C8 C20 122.41(16) . .
C11 C12 C7 118.69(19) . .
C11 C12 C23 120.15(17) . .
C7 C12 C23 121.01(17) . .
C10 C9 C8 121.0(2) . .
C9 C10 C11 119.88(18) . .
C10 C11 C12 121.36(18) . .
C14 C13 C18 119.97(17) . .
C14 C13 C2 121.08(17) . .
C18 C13 C2 118.95(16) . .
C15 C14 C13 119.3(2) . .
C15 C14 C26 119.26(18) . .
C13 C14 C26 121.19(16) . .
C16 C15 C14 120.7(2) . .
C15 C16 C17 120.2(2) . .
C16 C17 C18 120.9(2) . .
C17 C18 C13 118.9(2) . .
C17 C18 C29 118.9(2) . .
C13 C18 C29 122.18(17) . .
F2 C19 F3 105.90(18) . .
F2 C19 F4 106.16(17) . .
F3 C19 F4 105.80(17) . .
F2 C19 C4 112.75(16) . .
F3 C19 C4 113.41(16) . .
F4 C19 C4 112.22(18) . .
C8 C20 C22 109.88(16) . .
C8 C20 C21 112.23(18) . .
C22 C20 C21 110.20(18) . .
C12 C23 C24 113.1(2) . .
C12 C23 C25 110.43(17) . .
C24 C23 C25 110.2(2) . .
C14 C26 C27 113.10(19) . .
C14 C26 C28 109.18(18) . .
C27 C26 C28 110.38(19) . .
C31 C29 C18 110.6(2) . .
C31 C29 C30 108.4(2) . .
C18 C29 C30 113.36(19) . .
O1 C32 C33 104.21(18) . .
C34 C33 C32 101.21(19) . .
C33 C34 C35 104.41(17) . .
O1 C35 C34 105.49(18) . .
C37 C36 C41 117.9(3) . .
C37 C36 C42 119.7(4) . .
C41 C36 C42 122.3(4) . .
C36 C37 C38 120.5(3) . .
C39 C38 C37 120.7(4) . .
C38 C39 C40 118.6(3) . .
C41 C40 C39 120.4(3) . .
C40 C41 C36 121.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 F1 1.9698(14) .
Cr1 F1 2.0272(13) 2_666
Cr1 O1 2.0518(15) .
Cr1 C1 2.1167(19) .
F1 Cr1 2.0272(13) 2_666
F2 C19 1.336(2) .
F3 C19 1.339(2) .
F4 C19 1.343(2) .
O1 C32 1.461(3) .
O1 C35 1.464(3) .
C1 C2 1.420(2) .
C1 C6 1.423(2) .
C2 C3 1.399(3) .
C2 C13 1.508(2) .
C3 C4 1.389(2) .
C4 C5 1.390(3) .
C4 C19 1.493(3) .
C5 C6 1.397(3) .
C6 C7 1.507(2) .
C7 C8 1.408(3) .
C7 C12 1.421(2) .
C8 C9 1.406(3) .
C8 C20 1.516(3) .
C12 C11 1.398(3) .
C12 C23 1.517(3) .
C9 C10 1.380(3) .
C10 C11 1.387(3) .
C13 C14 1.413(3) .
C13 C18 1.418(3) .
C14 C15 1.399(3) .
C14 C26 1.517(3) .
C15 C16 1.389(4) .
C16 C17 1.390(4) .
C17 C18 1.400(3) .
C18 C29 1.531(3) .
C20 C22 1.535(3) .
C20 C21 1.536(3) .
C23 C24 1.532(3) .
C23 C25 1.538(4) .
C26 C27 1.528(3) .
C26 C28 1.534(3) .
C29 C31 1.521(4) .
C29 C30 1.537(3) .
C32 C33 1.520(3) .
C33 C34 1.510(3) .
C34 C35 1.520(3) .
C36 C37 1.372(5) .
C36 C41 1.379(6) .
C36 C42 1.504(5) .
C37 C38 1.397(4) .
C38 C39 1.368(6) .
C39 C40 1.382(7) .
C40 C41 1.366(7) .
