#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:30:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178716 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/27/4082749.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_4082749
loop_
_publ_author_name
'Kalz, Kai F.'
'Kindermann, Nicole'
'Xiang, Sheng-Qi'
'Kronz, Andreas'
'Lange, Adam'
'Meyer, Franc'
_publ_section_title
;
 Revisiting the Synthesis and Elucidating the Structure of Potassium
 Cyclopentadienyldicarbonylruthenate, K[CpRu(CO)2]
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1475
_journal_paper_doi               10.1021/om500107j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C7 H5 O2 Ru, C4 H8 O, K'
_chemical_formula_sum            'C11 H13 K O3 Ru'
_chemical_formula_weight         333.38
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.7374(17)
_cell_length_b                   11.492(2)
_cell_length_c                   24.169(5)
_cell_measurement_reflns_used    21384
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.705
_cell_measurement_theta_min      1.685
_cell_volume                     2426.8(8)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.705
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.7075
_exptl_absorpt_correction_T_min  0.2958
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0303P)²+0.6499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2029
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om500107j_si_002.cif
_cod_data_source_block           kk33
_cod_original_cell_volume        2426.9(8)
_cod_database_code               4082749
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.824
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.8591(3) 0.7228(2) 0.32590(9) 0.0222(5) Uani 1 1 d . .
C2 C 0.6384(3) 0.8578(2) 0.30693(9) 0.0223(5) Uani 1 1 d . .
C3 C 0.7874(3) 0.9681(2) 0.43285(10) 0.0248(5) Uani 1 1 d . .
H11 H 0.8188 1.0445 0.4231 0.030 Uiso 1 1 calc R U
C4 C 0.6334(3) 0.9272(2) 0.43682(10) 0.0306(6) Uani 1 1 d . .
H10 H 0.5442 0.9718 0.4292 0.037 Uiso 1 1 calc R U
C5 C 0.6357(3) 0.8091(2) 0.45394(10) 0.0316(6) Uani 1 1 d . .
H13 H 0.5491 0.7613 0.4608 0.038 Uiso 1 1 calc R U
C6 C 0.7917(3) 0.7757(2) 0.45892(9) 0.0251(5) Uani 1 1 d . .
H14 H 0.8280 0.7007 0.4691 0.030 Uiso 1 1 calc R U
C7 C 0.8842(3) 0.8742(2) 0.44605(9) 0.0212(5) Uani 1 1 d . .
H7 H 0.9929 0.8762 0.4463 0.025 Uiso 1 1 calc R U
C8 C 0.2827(3) 0.6953(2) 0.33648(11) 0.0259(5) Uani 1 1 d . .
H17A H 0.2090 0.7400 0.3138 0.031 Uiso 1 1 calc R U
H17B H 0.3824 0.7361 0.3360 0.031 Uiso 1 1 calc R U
C9 C 0.2241(3) 0.6830(2) 0.39559(12) 0.0296(6) Uani 1 1 d . .
H12A H 0.2634 0.7461 0.4196 0.035 Uiso 1 1 calc R U
H12B H 0.1109 0.6827 0.3969 0.035 Uiso 1 1 calc R U
C10 C 0.2896(3) 0.5657(2) 0.41222(11) 0.0281(6) Uani 1 1 d . .
H5A H 0.3981 0.5724 0.4236 0.034 Uiso 1 1 calc R U
H5B H 0.2300 0.5302 0.4427 0.034 Uiso 1 1 calc R U
C11 C 0.2736(3) 0.4964(3) 0.35928(11) 0.0271(5) Uani 1 1 d . .
H20A H 0.3502 0.4330 0.3579 0.032 Uiso 1 1 calc R U
H20B H 0.1700 0.4620 0.3565 0.032 Uiso 1 1 calc R U
O1 O 0.9254(2) 0.65534(16) 0.29830(7) 0.0311(4) Uani 1 1 d . .
O2 O 0.5668(2) 0.88016(16) 0.26696(7) 0.0333(4) Uani 1 1 d . .
O3 O 0.2991(2) 0.57826(13) 0.31514(7) 0.0237(4) Uani 1 1 d . .
K1 K 0.60823(5) 0.55105(4) 0.28016(2) 0.02198(13) Uani 1 1 d . .
Ru1 Ru 0.74822(2) 0.82312(2) 0.36864(2) 0.01690(10) Uani 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 '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
O1 C1 Ru1 177.3(2) . .
O1 C1 K1 74.34(14) . .
Ru1 C1 K1 102.99(9) . .
O2 C2 Ru1 179.8(2) . .
O2 C2 K1 92.88(15) . 8_765
Ru1 C2 K1 87.31(8) . 8_765
C7 C3 C4 107.4(2) . .
C7 C3 Ru1 71.80(13) . .
C4 C3 Ru1 70.57(13) . .
C5 C4 C3 108.7(2) . .
C5 C4 Ru1 72.61(14) . .
C3 C4 Ru1 73.02(13) . .
C4 C5 C6 107.3(2) . .
C4 C5 Ru1 71.13(14) . .
C6 C5 Ru1 71.56(13) . .
C5 C6 C7 108.1(2) . .
C5 C6 Ru1 72.21(13) . .
C7 C6 Ru1 72.29(13) . .
C3 C7 C6 108.5(2) . .
C3 C7 Ru1 72.54(13) . .
C6 C7 Ru1 71.37(13) . .
O3 C8 C9 106.33(19) . .
C10 C9 C8 101.8(2) . .
C11 C10 C9 102.0(2) . .
O3 C11 C10 105.6(2) . .
C1 O1 K1 164.51(18) . 6_656
C1 O1 K1 83.88(14) . .
K1 O1 K1 104.90(6) 6_656 .
C2 O2 K1 142.50(16) . 3_655
C11 O3 C8 109.13(18) . .
C11 O3 K1 107.16(14) . .
C8 O3 K1 107.56(14) . .
C11 O3 K1 115.79(14) . 6_556
C8 O3 K1 109.31(14) . 6_556
K1 O3 K1 107.57(6) . 6_556
O2 K1 O1 72.64(6) 3_645 6_556
O2 K1 O3 70.87(5) 3_645 .
O1 K1 O3 66.82(5) 6_556 .
O2 K1 O3 93.97(5) 3_645 6_656
O1 K1 O3 74.71(5) 6_556 6_656
O3 K1 O3 141.26(5) . 6_656
O2 K1 O1 148.12(5) 3_645 .
O1 K1 O1 117.06(6) 6_556 .
O3 K1 O1 140.87(5) . .
O3 K1 O1 62.83(5) 6_656 .
O2 K1 C1 169.85(6) 3_645 .
O1 K1 C1 111.89(6) 6_556 .
O3 K1 C1 119.15(6) . .
O3 K1 C1 78.96(6) 6_656 .
O1 K1 C1 21.77(5) . .
O2 K1 C2 88.44(6) 3_645 8_755
O1 K1 C2 147.37(6) 6_556 8_755
O3 K1 C2 132.22(6) . 8_755
O3 K1 C2 80.53(5) 6_656 8_755
O1 K1 C2 67.38(6) . 8_755
C1 K1 C2 83.25(6) . 8_755
O2 K1 Ru1 85.41(4) 3_645 8_755
O1 K1 Ru1 157.83(4) 6_556 8_755
O3 K1 Ru1 103.51(4) . 8_755
O3 K1 Ru1 110.74(4) 6_656 8_755
O1 K1 Ru1 83.35(4) . 8_755
C1 K1 Ru1 90.28(4) . 8_755
C2 K1 Ru1 30.23(4) 8_755 8_755
O2 K1 Ru1 163.48(4) 3_645 .
O1 K1 Ru1 101.91(4) 6_556 .
O3 K1 Ru1 92.62(4) . .
O3 K1 Ru1 99.65(4) 6_656 .
O1 K1 Ru1 48.33(3) . .
C1 K1 Ru1 26.56(4) . .
C2 K1 Ru1 102.93(4) 8_755 .
Ru1 K1 Ru1 98.342(18) 8_755 .
O2 K1 K1 113.48(4) 3_645 6_656
O1 K1 K1 109.42(4) 6_556 6_656
O3 K1 K1 173.61(3) . 6_656
O3 K1 K1 36.12(4) 6_656 6_656
O1 K1 K1 35.30(3) . 6_656
C1 K1 K1 56.70(4) . 6_656
C2 K1 K1 53.71(4) 8_755 6_656
Ru1 K1 K1 81.824(12) 8_755 6_656
Ru1 K1 K1 83.024(10) . 6_656
O2 K1 K1 48.57(4) 3_645 6_556
O1 K1 K1 39.80(4) 6_556 6_556
O3 K1 K1 36.31(4) . 6_556
O3 K1 K1 107.34(4) 6_656 6_556
O1 K1 K1 155.11(4) . 6_556
C1 K1 K1 140.46(4) . 6_556
C2 K1 K1 136.04(4) 8_755 6_556
Ru1 K1 K1 121.167(11) 8_755 6_556
Ru1 K1 K1 117.483(10) . 6_556
K1 K1 K1 143.10(3) 6_656 6_556
C2 Ru1 C1 87.40(10) . .
C2 Ru1 C4 104.27(10) . .
C1 Ru1 C4 167.90(10) . .
C2 Ru1 C6 157.71(10) . .
C1 Ru1 C6 107.56(10) . .
C4 Ru1 C6 60.35(9) . .
C2 Ru1 C5 121.84(10) . .
C1 Ru1 C5 133.85(10) . .
C4 Ru1 C5 36.26(10) . .
C6 Ru1 C5 36.23(9) . .
C2 Ru1 C7 152.48(10) . .
C1 Ru1 C7 110.37(9) . .
C4 Ru1 C7 60.12(9) . .
C6 Ru1 C7 36.34(8) . .
C5 Ru1 C7 60.38(9) . .
C2 Ru1 C3 118.22(10) . .
C1 Ru1 C3 139.38(9) . .
C4 Ru1 C3 36.41(9) . .
C6 Ru1 C3 60.23(9) . .
C5 Ru1 C3 60.51(9) . .
C7 Ru1 C3 35.66(9) . .
C2 Ru1 K1 62.46(7) . 8_765
C1 Ru1 K1 86.49(7) . 8_765
C4 Ru1 K1 101.61(7) . 8_765
C6 Ru1 K1 133.08(6) . 8_765
C5 Ru1 K1 137.24(7) . 8_765
C7 Ru1 K1 96.75(6) . 8_765
C3 Ru1 K1 79.77(7) . 8_765
C2 Ru1 K1 64.49(7) . .
C1 Ru1 K1 50.46(7) . .
C4 Ru1 K1 131.92(7) . .
C6 Ru1 K1 112.16(6) . .
C5 Ru1 K1 107.26(7) . .
C7 Ru1 K1 143.02(6) . .
C3 Ru1 K1 167.47(6) . .
K1 Ru1 K1 111.025(19) 8_765 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.175(3) .
C1 Ru1 1.826(2) .
C1 K1 3.150(2) .
C2 O2 1.179(3) .
C2 Ru1 1.818(2) .
C2 K1 3.202(2) 8_765
C3 C7 1.407(3) .
C3 C4 1.429(4) .
C3 Ru1 2.303(2) .
C4 C5 1.419(4) .
C4 Ru1 2.270(2) .
C5 C6 1.421(4) .
C5 Ru1 2.290(2) .
C6 C7 1.426(3) .
C6 Ru1 2.281(2) .
C7 Ru1 2.293(2) .
C8 O3 1.447(3) .
C8 C9 1.524(4) .
C9 C10 1.519(4) .
C10 C11 1.513(4) .
C11 O3 1.439(3) .
O1 K1 2.7539(18) 6_656
O1 K1 3.0507(19) .
O2 K1 2.7374(18) 3_655
O3 K1 2.8478(19) .
O3 K1 2.8605(19) 6_556
K1 O2 2.7374(18) 3_645
K1 O1 2.7539(18) 6_556
K1 O3 2.8605(19) 6_656
K1 C2 3.202(2) 8_755
K1 Ru1 3.6066(7) 8_755
K1 Ru1 3.9806(8) .
K1 K1 4.6054(9) 6_656
K1 K1 4.6054(9) 6_556
Ru1 K1 3.6067(7) 8_765
