#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:28:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179972 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/66/7026654.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_7026654
loop_
_publ_author_name
'Murugesapandian, Balasubramanian'
'Roesky, Peter W.'
_publ_section_title
;
 Sodium and potassium compounds of [(η(6)-benzenecarboxylate)Cr(CO)(3)]
 and [(η(6)-1,4-benzenedicarboxylate)Cr(CO)(3)].
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9598
_journal_page_last               9603
_journal_paper_doi               10.1039/c0dt00569j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C11 H16 Cr Na2 O13'
_chemical_formula_sum            'C11 H16 Cr Na2 O13'
_chemical_formula_weight         454.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.384(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1130(5)
_cell_length_b                   22.6678(19)
_cell_length_c                   12.6748(11)
_cell_measurement_reflns_used    17989
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.67
_cell_measurement_theta_min      1.80
_cell_volume                     1745.4(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e/3'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17690
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.6982
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment from plate'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0321
_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)+(0.0455P)²+0.3603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                4044
_reflns_number_total             4694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00569j.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7026654
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.0769(2) 0.22439(6) 0.70304(11) 0.0218(3) Uani 1 1 d .
C2 C -0.0673(2) 0.27151(6) 0.67251(12) 0.0226(3) Uani 1 1 d .
H2 H -0.2180 0.2635 0.6504 0.027 Uiso 1 1 calc R
C3 C 0.0091(2) 0.33063(6) 0.67434(11) 0.0227(3) Uani 1 1 d .
H3 H -0.0904 0.3620 0.6552 0.027 Uiso 1 1 calc R
C4 C 0.2338(2) 0.34243(6) 0.70472(11) 0.0216(3) Uani 1 1 d .
C5 C 0.3779(2) 0.29520(6) 0.73806(11) 0.0221(3) Uani 1 1 d .
H5 H 0.5280 0.3032 0.7616 0.027 Uiso 1 1 calc R
C6 C 0.3014(2) 0.23694(6) 0.73655(11) 0.0225(3) Uani 1 1 d .
H6 H 0.4001 0.2057 0.7580 0.027 Uiso 1 1 calc R
C7 C -0.0094(2) 0.16159(6) 0.69908(12) 0.0238(3) Uani 1 1 d .
C8 C 0.3259(2) 0.40470(6) 0.69940(11) 0.0233(3) Uani 1 1 d .
C9 C 0.3799(3) 0.32570(7) 0.50358(12) 0.0257(3) Uani 1 1 d .
C10 C 0.3318(3) 0.21021(7) 0.51792(12) 0.0280(3) Uani 1 1 d .
C11 C -0.0115(3) 0.27364(8) 0.46384(12) 0.0297(3) Uani 1 1 d .
O1 O 0.11637(19) 0.12272(5) 0.74406(10) 0.0309(2) Uani 1 1 d .
O2 O -0.19823(19) 0.15288(5) 0.65326(10) 0.0323(2) Uani 1 1 d .
O3 O 0.20127(19) 0.44359(5) 0.65362(10) 0.0291(2) Uani 1 1 d .
O4 O 0.52009(19) 0.41230(5) 0.73995(9) 0.0296(2) Uani 1 1 d .
O5 O 0.4844(2) 0.35848(6) 0.46081(11) 0.0387(3) Uani 1 1 d .
O6 O 0.3990(3) 0.16884(6) 0.48041(11) 0.0452(3) Uani 1 1 d .
O7 O -0.1568(2) 0.27037(8) 0.39845(11) 0.0489(4) Uani 1 1 d .
O8 O 0.9675(2) 0.50633(6) 0.80657(10) 0.0293(2) Uani 1 1 d .
O9 O 0.8380(3) 0.39544(7) 0.94699(15) 0.0454(3) Uani 1 1 d .
O10 O 0.7142(2) 0.53598(6) 1.03842(11) 0.0329(3) Uani 1 1 d .
O11 O 0.4777(2) 0.56911(5) 0.77664(10) 0.0290(2) Uani 1 1 d .
O12 O 0.0017(2) 0.56986(6) 0.56943(11) 0.0314(2) Uani 1 1 d .
O13 O 0.3193(2) 0.51907(6) 0.41554(10) 0.0305(2) Uani 1 1 d .
Na1 Na 0.62551(11) 0.48158(3) 0.87916(5) 0.02979(14) Uani 1 1 d .
Na2 Na 0.36097(10) 0.53755(3) 0.59929(5) 0.02771(14) Uani 1 1 d .
Cr1 Cr 0.20894(4) 0.275886(9) 0.576484(18) 0.01920(7) Uani 1 1 d .
H8A H 0.963(4) 0.5405(12) 0.789(2) 0.049(7) Uiso 1 1 d .
H8B H 1.034(5) 0.4907(12) 0.762(2) 0.055(7) Uiso 1 1 d .
H9A H 0.813(4) 0.3820(12) 1.003(2) 0.051(7) Uiso 1 1 d .
H9B H 0.790(7) 0.372(2) 0.905(4) 0.116(16) Uiso 1 1 d .
H10A H 0.812(5) 0.5225(13) 1.076(2) 0.055(8) Uiso 1 1 d .
H10B H 0.750(5) 0.5652(15) 1.032(3) 0.070(10) Uiso 1 1 d .
H11A H 0.592(4) 0.5887(12) 0.773(2) 0.051(7) Uiso 1 1 d .
H11B H 0.393(4) 0.5908(11) 0.7975(19) 0.041(6) Uiso 1 1 d .
H12A H -0.048(4) 0.5928(10) 0.6079(19) 0.036(6) Uiso 1 1 d .
H12B H -0.027(5) 0.5741(13) 0.510(2) 0.059(8) Uiso 1 1 d .
H13A H 0.214(4) 0.5013(11) 0.4046(18) 0.039(6) Uiso 1 1 d .
H13B H 0.334(4) 0.5373(11) 0.370(2) 0.037(6) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 '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 118.95(13) . .
C2 C1 C7 119.80(13) . .
C6 C1 C7 121.25(13) . .
C2 C1 Cr1 70.63(8) . .
C6 C1 Cr1 72.06(8) . .
C7 C1 Cr1 128.75(10) . .
C1 C2 C3 121.06(13) . .
C1 C2 Cr1 71.94(8) . .
C3 C2 Cr1 72.16(8) . .
C4 C3 C2 119.51(13) . .
C4 C3 Cr1 71.22(8) . .
C2 C3 Cr1 70.29(8) . .
C3 C4 C5 119.43(13) . .
C3 C4 C8 121.12(13) . .
C5 C4 C8 119.42(13) . .
C3 C4 Cr1 71.61(8) . .
C5 C4 Cr1 72.19(8) . .
C8 C4 Cr1 126.52(9) . .
C6 C5 C4 120.75(13) . .
C6 C5 Cr1 71.49(8) . .
C4 C5 Cr1 70.52(8) . .
C5 C6 C1 120.23(13) . .
C5 C6 Cr1 71.89(8) . .
C1 C6 Cr1 70.60(8) . .
O2 C7 O1 125.76(14) . .
O2 C7 C1 117.62(13) . .
O1 C7 C1 116.62(13) . .
O4 C8 O3 126.04(14) . .
O4 C8 C4 116.57(13) . .
O3 C8 C4 117.39(13) . .
O5 C9 Cr1 177.32(14) . .
O6 C10 Cr1 177.16(16) . .
O7 C11 Cr1 175.41(16) . .
C8 O3 Na2 119.51(10) . .
C8 O4 Na1 123.88(10) . .
C9 O5 Na2 158.54(12) . 3_666
Na1 O10 Na1 98.82(5) . 3_667
Na2 O11 Na1 107.80(5) . .
Na2 O13 Na2 100.14(5) . 3_666
O10 Na1 O4 169.40(6) . .
O10 Na1 O8 94.41(5) . .
O4 Na1 O8 92.56(5) . .
O10 Na1 O9 93.07(6) . .
O4 Na1 O9 79.89(6) . .
O8 Na1 O9 82.67(5) . .
O10 Na1 O10 81.18(5) . 3_667
O4 Na1 O10 92.07(5) . 3_667
O8 Na1 O10 175.23(5) . 3_667
O9 Na1 O10 99.31(6) . 3_667
O10 Na1 O11 93.73(5) . .
O4 Na1 O11 94.93(5) . .
O8 Na1 O11 84.05(5) . .
O9 Na1 O11 165.50(6) . .
O10 Na1 O11 94.38(5) 3_667 .
O10 Na1 Na1 41.43(4) . 3_667
O4 Na1 Na1 131.32(4) . 3_667
O8 Na1 Na1 135.81(4) . 3_667
O9 Na1 Na1 98.22(5) . 3_667
O10 Na1 Na1 39.75(3) 3_667 3_667
O11 Na1 Na1 95.35(4) . 3_667
O10 Na1 Na2 129.02(4) . .
O4 Na1 Na2 59.90(3) . .
O8 Na1 Na2 82.51(4) . .
O9 Na1 Na2 136.19(5) . .
O10 Na1 Na2 98.81(4) 3_667 .
O11 Na1 Na2 35.29(3) . .
Na1 Na1 Na2 120.66(3) 3_667 .
O12 Na2 O13 84.13(5) . .
O12 Na2 O13 160.12(6) . 3_666
O13 Na2 O13 79.86(5) . 3_666
O12 Na2 O11 103.80(5) . .
O13 Na2 O11 166.48(6) . .
O13 Na2 O11 94.26(5) 3_666 .
O12 Na2 O3 85.46(5) . .
O13 Na2 O3 96.87(5) . .
O13 Na2 O3 84.84(5) 3_666 .
O11 Na2 O3 94.69(5) . .
O12 Na2 O5 91.93(5) . 3_666
O13 Na2 O5 82.99(5) . 3_666
O13 Na2 O5 97.70(5) 3_666 3_666
O11 Na2 O5 85.78(5) . 3_666
O3 Na2 O5 177.39(5) . 3_666
O12 Na2 Na2 123.24(5) . 3_666
O13 Na2 Na2 40.05(3) . 3_666
O13 Na2 Na2 39.82(3) 3_666 3_666
O11 Na2 Na2 132.92(4) . 3_666
O3 Na2 Na2 91.09(4) . 3_666
O5 Na2 Na2 90.47(4) 3_666 3_666
O12 Na2 Na1 122.54(4) . .
O13 Na2 Na1 145.32(4) . .
O13 Na2 Na1 68.69(4) 3_666 .
O11 Na2 Na1 36.91(3) . .
O3 Na2 Na1 66.87(3) . .
O5 Na2 Na1 114.61(4) 3_666 .
Na2 Na2 Na1 107.30(3) 3_666 .
C11 Cr1 C9 91.98(7) . .
C11 Cr1 C10 87.81(7) . .
C9 Cr1 C10 90.79(7) . .
C11 Cr1 C2 83.53(6) . .
C9 Cr1 C2 144.75(6) . .
C10 Cr1 C2 123.79(6) . .
C11 Cr1 C1 104.60(6) . .
C9 Cr1 C1 162.98(6) . .
C10 Cr1 C1 93.63(6) . .
C2 Cr1 C1 37.42(5) . .
C11 Cr1 C4 124.78(6) . .
C9 Cr1 C4 87.39(6) . .
C10 Cr1 C4 147.40(6) . .
C2 Cr1 C4 67.46(5) . .
C1 Cr1 C4 80.06(5) . .
C11 Cr1 C3 92.73(6) . .
C9 Cr1 C3 108.33(6) . .
C10 Cr1 C3 160.84(6) . .
C2 Cr1 C3 37.55(5) . .
C1 Cr1 C3 67.69(5) . .
C4 Cr1 C3 37.17(5) . .
C11 Cr1 C6 141.32(6) . .
C9 Cr1 C6 126.56(6) . .
C10 Cr1 C6 88.48(6) . .
C2 Cr1 C6 67.00(5) . .
C1 Cr1 C6 37.34(5) . .
C4 Cr1 C6 67.10(5) . .
C3 Cr1 C6 79.16(5) . .
C11 Cr1 C5 159.33(6) . .
C9 Cr1 C5 96.25(6) . .
C10 Cr1 C5 110.93(6) . .
C2 Cr1 C5 78.81(5) . .
C1 Cr1 C5 66.83(5) . .
C4 Cr1 C5 37.29(5) . .
C3 Cr1 C5 66.69(5) . .
C6 Cr1 C5 36.61(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.411(2) .
C1 C6 1.420(2) .
C1 C7 1.5169(19) .
C1 Cr1 2.2080(14) .
C2 C3 1.4185(19) .
C2 Cr1 2.1910(14) .
C3 C4 1.410(2) .
C3 Cr1 2.2154(14) .
C4 C5 1.421(2) .
C4 C8 1.5239(19) .
C4 Cr1 2.2103(14) .
C5 C6 1.4006(19) .
C5 Cr1 2.2322(15) .
C6 Cr1 2.2270(14) .
C7 O2 1.2490(19) .
C7 O1 1.2627(19) .
C8 O4 1.2520(19) .
C8 O3 1.2633(18) .
C9 O5 1.1541(19) .
C9 Cr1 1.8534(15) .
C10 O6 1.148(2) .
C10 Cr1 1.8589(16) .
C11 O7 1.148(2) .
C11 Cr1 1.8518(17) .
O3 Na2 2.4724(13) .
O4 Na1 2.3963(13) .
O5 Na2 2.6809(14) 3_666
O8 Na1 2.4413(14) .
O9 Na1 2.4476(17) .
O10 Na1 2.3761(15) .
O10 Na1 2.4585(15) 3_667
O11 Na2 2.3911(14) .
O11 Na1 2.4860(14) .
O12 Na2 2.3062(14) .
O13 Na2 2.3522(14) .
O13 Na2 2.3634(14) 3_666
Na1 O10 2.4585(15) 3_667
Na1 Na1 3.6717(13) 3_667
Na1 Na2 3.9410(10) .
Na2 O13 2.3633(14) 3_666
Na2 O5 2.6809(14) 3_666
Na2 Na2 3.6159(13) 3_666
