#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:36:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178907 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/36/4113699.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_4113699
loop_
_publ_author_name
'F. Albert Cotton'
'James P. Donahue'
'Carlos A. Murillo'
_publ_section_title
;
 Polyunsaturated Dicarboxylate Tethers Connecting Dimolybdenum Redox and
 Chromophoric Centers: Syntheses, Structures, and Electrochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5436
_journal_page_last               5450
_journal_paper_doi               10.1021/ja029101i
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'H3 C O C (O) (C H = C H)4 C (O) O C H3'
_chemical_formula_sum            'C12 H14 O4'
_chemical_formula_weight         222.23
_chemical_name_common            'texic acid dimethyl ester'
_chemical_name_systematic
;
 Deca-trans,trans,trans,trans-2:4:6:8-tetraene-1,10-dioic acid
 dimethyl ester
;
_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                104.439(4)
_cell_angle_beta                 94.001(4)
_cell_angle_gamma                104.544(4)
_cell_formula_units_Z            1
_cell_length_a                   5.9286(12)
_cell_length_b                   6.6599(13)
_cell_length_c                   7.7447(16)
_cell_measurement_reflns_used    959
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.507
_cell_measurement_theta_min      2.744
_cell_volume                     283.77(10)
_computing_cell_refinement       'SAINT V. 6.22'
_computing_data_collection       'SMART V. 5.618'
_computing_data_reduction        'SAINT V. 6.22'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       'Bruker SMART 1000'
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       'omega 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  0.0082
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1979
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.74
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.9576
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       column
_exptl_crystal_F_000             118
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0548P)²+0.0534P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                976
_reflns_number_total             1236
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja029101isi20030123_021228_06.cif
_cod_data_source_block           xl
_cod_database_code               4113699
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
O1 O 0.82235(17) 1.16575(17) 0.45562(13) 0.0434(3) Uani 1 1 d .
O2 O 1.08114(15) 1.14709(16) 0.25823(12) 0.0353(3) Uani 1 1 d .
C1 C 1.2597(2) 1.3081(2) 0.39386(19) 0.0387(4) Uani 1 1 d .
H1A H 1.4067 1.3390 0.3449 0.058 Uiso 1 1 calc R
H1B H 1.2816 1.2543 0.4975 0.058 Uiso 1 1 calc R
H1C H 1.2107 1.4390 0.4303 0.058 Uiso 1 1 calc R
C2 C 0.8670(2) 1.0891(2) 0.30822(17) 0.0285(3) Uani 1 1 d .
C3 C 0.7011(2) 0.9224(2) 0.15976(17) 0.0297(3) Uani 1 1 d .
C4 C 0.4803(2) 0.8332(2) 0.18278(17) 0.0288(3) Uani 1 1 d .
C5 C 0.3082(2) 0.6701(2) 0.04401(18) 0.0300(3) Uani 1 1 d .
C6 C 0.0872(2) 0.5812(2) 0.06896(17) 0.0296(3) Uani 1 1 d .
H1 H 0.764(2) 0.881(2) 0.0373(19) 0.025(3) Uiso 1 1 d .
H2 H 0.429(2) 0.875(2) 0.292(2) 0.031(4) Uiso 1 1 d .
H5 H 0.358(3) 0.627(2) -0.071(2) 0.036(4) Uiso 1 1 d .
H6 H 0.038(3) 0.625(2) 0.181(2) 0.035(4) Uiso 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0359(6) 0.0456(7) 0.0342(6) -0.0046(4) 0.0068(4) 0.0003(5)
O2 0.0248(5) 0.0384(6) 0.0322(5) 0.0026(4) 0.0010(4) -0.0019(4)
C1 0.0270(7) 0.0375(8) 0.0396(8) 0.0043(6) -0.0045(6) -0.0038(6)
C2 0.0259(7) 0.0280(7) 0.0297(6) 0.0075(5) 0.0025(5) 0.0052(5)
C3 0.0270(7) 0.0297(7) 0.0275(6) 0.0042(5) 0.0003(5) 0.0038(5)
C4 0.0266(7) 0.0283(7) 0.0283(7) 0.0048(5) 0.0006(5) 0.0059(5)
C5 0.0274(7) 0.0296(7) 0.0295(7) 0.0054(5) -0.0005(5) 0.0055(5)
C6 0.0272(7) 0.0286(7) 0.0297(7) 0.0052(6) 0.0000(5) 0.0059(5)
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'
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_3
_geom_angle_publ_flag
C2 O2 C1 115.78(10) . y
O1 C2 O2 123.18(12) . y
O1 C2 C3 126.05(12) . y
O2 C2 C3 110.78(10) . y
C4 C3 C2 120.95(12) . y
C3 C4 C5 124.10(12) . y
C6 C5 C4 123.54(13) . y
C5 C6 C6 124.12(16) 2_565 y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.2055(16) . y
O2 C2 1.3445(15) . y
O2 C1 1.4445(16) . y
C2 C3 1.4762(17) . y
C3 C4 1.3390(18) . y
C4 C5 1.4436(18) . y
C5 C6 1.3445(19) . y
C6 C6 1.445(2) 2_565 y
