#------------------------------------------------------------------------------
#$Date: 2019-11-08 03:14:48 +0200 (Fri, 08 Nov 2019) $
#$Revision: 225010 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/80/7058028.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_7058028
loop_
_publ_author_name
'Xu, Lei'
'Jiang, Liping'
'Li, Shasha'
'Zhang, Guofang'
'Zhang, Weiqiang'
'Gao, Ziwei'
_publ_section_title
;
 Unexpected formation and conversion: role of substituents of 1,3-ynones
 in the reactivity and product distribution during their reactions with
 Ru3(CO)12
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1478
_journal_paper_doi               10.1039/C8NJ05573D
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C14 H6 O12 Ru2'
_chemical_formula_weight         568.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-03 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.958(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.385(5)
_cell_length_b                   11.395(3)
_cell_length_c                   11.933(4)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.37
_cell_volume                     1786.9(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.366
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.113
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6139
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0154P)²+3.1504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1553
_reflns_number_total             1758
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj05573d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7058027--7058034.cif.'
_cod_database_code               7058028
_shelx_shelxl_version_number     2014/7
_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   0.791
_shelx_estimated_absorpt_t_max   0.844
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ru1 Ru 0.10623(2) 0.11889(2) 0.80313(2) 0.01425(8) Uani 1 1 d . .
O1 O 0.04589(15) 0.47304(16) 0.87310(18) 0.0239(5) Uani 1 1 d . .
O2 O 0.19344(17) 0.41921(19) 0.8241(2) 0.0383(6) Uani 1 1 d . .
O3 O 0.04894(17) 0.11736(18) 1.04046(18) 0.0288(5) Uani 1 1 d . .
O4 O 0.13046(18) -0.15264(18) 0.79821(18) 0.0315(5) Uani 1 1 d . .
O5 O 0.16407(17) 0.1665(2) 0.56895(19) 0.0354(5) Uani 1 1 d . .
O6 O 0.32776(17) 0.1715(2) 0.9105(2) 0.0363(6) Uani 1 1 d . .
C1 C 0.0934(3) 0.5821(3) 0.9182(3) 0.0380(9) Uani 1 1 d . .
H1A H 0.0446 0.6287 0.9509 0.057 Uiso 1 1 calc R U
H1B H 0.1529 0.5646 0.9776 0.057 Uiso 1 1 calc R U
H1C H 0.1150 0.6264 0.8565 0.057 Uiso 1 1 calc R U
C2 C 0.1050(2) 0.4000(2) 0.8252(2) 0.0207(6) Uani 1 1 d . .
C3 C 0.0469(2) 0.2928(2) 0.7811(2) 0.0177(6) Uani 1 1 d . .
C4 C 0.0666(2) 0.1160(2) 0.9513(3) 0.0199(6) Uani 1 1 d . .
C5 C 0.1233(2) -0.0543(3) 0.7993(2) 0.0207(6) Uani 1 1 d . .
C6 C 0.1396(2) 0.1448(2) 0.6524(3) 0.0216(6) Uani 1 1 d . .
C7 C 0.2453(2) 0.1554(2) 0.8709(3) 0.0217(6) 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'
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
C7 Ru1 C4 91.76(12) . .
C7 Ru1 C6 88.98(12) . .
C4 Ru1 C6 171.90(11) . .
C7 Ru1 C5 96.76(11) . .
C4 Ru1 C5 93.26(11) . .
C6 Ru1 C5 94.66(11) . .
C7 Ru1 C3 99.13(11) . .
C4 Ru1 C3 88.18(11) . .
C6 Ru1 C3 83.74(11) . .
C5 Ru1 C3 164.00(11) . .
C7 Ru1 Ru1 167.54(8) . 2_556
C4 Ru1 Ru1 89.03(8) . 2_556
C6 Ru1 Ru1 88.53(8) . 2_556
C5 Ru1 Ru1 95.61(8) . 2_556
C3 Ru1 Ru1 68.46(7) . 2_556
C2 O1 C1 115.7(2) . .
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O2 C2 O1 123.3(3) . .
O2 C2 C3 126.3(3) . .
O1 C2 C3 110.3(2) . .
C3 C3 C2 124.82(15) 2_556 .
C3 C3 Ru1 111.00(8) 2_556 .
C2 C3 Ru1 124.1(2) . .
O3 C4 Ru1 175.8(2) . .
O4 C5 Ru1 178.1(3) . .
O5 C6 Ru1 174.6(3) . .
O6 C7 Ru1 176.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 C7 1.929(3) .
Ru1 C4 1.941(3) .
Ru1 C6 1.957(3) .
Ru1 C5 1.988(3) .
Ru1 C3 2.133(3) .
Ru1 Ru1 2.8850(10) 2_556
O1 C2 1.348(3) .
O1 C1 1.452(3) .
O2 C2 1.206(3) .
O3 C4 1.133(4) .
O4 C5 1.125(4) .
O5 C6 1.133(4) .
O6 C7 1.129(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.489(4) .
C3 C3 1.331(6) 2_556
