#------------------------------------------------------------------------------
#$Date: 2015-10-14 03:57:44 +0200 (Wed 14 de Oct de 2015) $
#$Revision: 167923 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/02/2020211.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2020211
loop_
_publ_author_name
'Jimenez, Jorge'
'Chakraborty, Indranil'
'Mascharak, Pradip'
_publ_section_title
;
 Synthesis and structures of ruthenium di- and tricarbonyl complexes
 derived from 4,5-diazafluoren-9-one
;
_journal_coeditor_code           OV3067
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615018100
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ru Cl2 (C11 H6 N2 O) (C O)2]'
_chemical_formula_moiety         'C13 H6 Cl2 N2 O3 Ru'
_chemical_formula_sum            'C13 H6 Cl2 N2 O3 Ru'
_chemical_formula_weight         410.17
_chemical_name_systematic
trans-Dicarbonyldichlorido(4,5-diazafluoren-9-one-κ²N,N')ruthenium(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.69
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5589(2)
_cell_length_b                   16.9199(6)
_cell_length_c                   12.7585(5)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.41
_cell_volume                     1391.31(8)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Bruker 2008) and OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13644
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.353
_diffrn_reflns_theta_min         2.022
_exptl_absorpt_coefficient_mu    1.520
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.419
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0290
_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)+(0.0393P)²+1.2351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                2598
_reflns_number_total             2840
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ov3067sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1391.30(8)
_cod_database_code               2020211
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Ru Ru1 0.70714(3) 0.37385(2) 0.63595(2) 0.03500(10) Uani d 1
Cl Cl1 0.94807(12) 0.34857(5) 0.79811(6) 0.05222(19) Uani d 1
Cl Cl2 0.49226(13) 0.38504(5) 0.46405(7) 0.0547(2) Uani d 1
O O3 0.7415(4) 0.01600(13) 0.5327(3) 0.0766(8) Uani d 1
O O2 0.9657(4) 0.51454(14) 0.6069(2) 0.0628(6) Uani d 1
O O1 0.4360(5) 0.47572(18) 0.7402(2) 0.0803(8) Uani d 1
N N1 0.5457(3) 0.26370(14) 0.66326(18) 0.0392(5) Uani d 1
N N2 0.8830(3) 0.29170(13) 0.55820(17) 0.0352(5) Uani d 1
C C3 0.3910(4) 0.2398(2) 0.7137(2) 0.0481(7) Uani d 1
H H3 0.3207 0.2775 0.7465 0.058 Uiso calc 1
C C4 0.3349(5) 0.1611(2) 0.7178(2) 0.0564(8) Uani d 1
H H4 0.2307 0.1473 0.7548 0.068 Uiso calc 1
C C5 0.4305(5) 0.1020(2) 0.6679(3) 0.0590(9) Uani d 1
H H5 0.3912 0.0493 0.6699 0.071 Uiso calc 1
C C6 0.5859(5) 0.12555(16) 0.6158(3) 0.0489(7) Uani d 1
C C7 0.6332(4) 0.20550(16) 0.6183(2) 0.0401(6) Uani d 1
C C9 0.8043(4) 0.21970(15) 0.5641(2) 0.0373(6) Uani d 1
C C13 1.0409(4) 0.29571(17) 0.5048(2) 0.0396(6) Uani d 1
H H13 1.1021 0.3445 0.4978 0.048 Uiso calc 1
C C12 1.1159(4) 0.23020(18) 0.4600(2) 0.0446(6) Uani d 1
H H12 1.2257 0.2360 0.4239 0.054 Uiso calc 1
C C11 1.0311(5) 0.15600(19) 0.4678(2) 0.0474(7) Uani d 1
H H11 1.0814 0.1117 0.4378 0.057 Uiso calc 1
C C10 0.8679(4) 0.15088(17) 0.5223(2) 0.0434(6) Uani d 1
C C8 0.7321(5) 0.08520(17) 0.5532(3) 0.0531(8) Uani d 1
C C2 0.8658(5) 0.46283(17) 0.6145(2) 0.0431(6) Uani d 1
C C1 0.5301(5) 0.43934(19) 0.7038(3) 0.0514(7) Uani d 1
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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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_publ_flag
C2 Ru1 C1 90.05(13) y
C2 Ru1 N2 95.24(10) y
C1 Ru1 N2 174.48(11) y
C2 Ru1 N1 175.16(10) y
C1 Ru1 N1 93.90(11) y
N2 Ru1 N1 80.89(8) y
C2 Ru1 Cl2 92.93(9) y
C1 Ru1 Cl2 93.72(10) y
N2 Ru1 Cl2 84.47(6) y
N1 Ru1 Cl2 89.61(6) y
C2 Ru1 Cl1 88.54(9) y
C1 Ru1 Cl1 94.06(10) y
N2 Ru1 Cl1 87.65(6) y
N1 Ru1 Cl1 88.39(6) y
Cl2 Ru1 Cl1 172.08(3) y
C7 N1 C3 114.0(3) ?
C7 N1 Ru1 107.51(17) ?
C3 N1 Ru1 138.5(2) ?
C9 N2 C13 114.8(2) ?
C9 N2 Ru1 108.51(16) ?
C13 N2 Ru1 136.70(18) ?
N1 C3 C4 122.0(3) ?
N1 C3 H3 119.0 ?
C4 C3 H3 119.0 ?
C3 C4 C5 121.8(3) ?
C3 C4 H4 119.1 ?
C5 C4 H4 119.1 ?
C6 C5 C4 116.7(3) ?
C6 C5 H5 121.6 ?
C4 C5 H5 121.6 ?
C5 C6 C7 117.0(3) ?
C5 C6 C8 136.2(3) ?
C7 C6 C8 106.8(3) ?
N1 C7 C6 128.5(3) ?
N1 C7 C9 121.5(2) ?
C6 C7 C9 110.0(3) ?
N2 C9 C10 127.1(3) ?
N2 C9 C7 121.6(2) ?
C10 C9 C7 111.3(2) ?
N2 C13 C12 122.5(3) ?
N2 C13 H13 118.7 ?
C12 C13 H13 118.7 ?
C13 C12 C11 121.4(3) ?
C13 C12 H12 119.3 ?
C11 C12 H12 119.3 ?
C12 C11 C10 116.8(3) ?
C12 C11 H11 121.6 ?
C10 C11 H11 121.6 ?
C9 C10 C11 117.4(3) ?
C9 C10 C8 106.5(3) ?
C11 C10 C8 136.1(3) ?
O3 C8 C6 127.9(3) ?
O3 C8 C10 126.8(3) ?
C6 C8 C10 105.4(2) ?
O2 C2 Ru1 176.3(3) ?
O1 C1 Ru1 178.9(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 C2 1.879(3) y
Ru1 C1 1.923(3) y
Ru1 N2 2.161(2) y
Ru1 N1 2.203(2) y
Ru1 Cl2 2.3844(9) y
Ru1 Cl1 2.3974(8) y
O3 C8 1.204(4) ?
O2 C2 1.108(4) ?
O1 C1 1.040(4) ?
N1 C7 1.323(4) ?
N1 C3 1.360(3) ?
N2 C9 1.330(3) ?
N2 C13 1.343(3) ?
C3 C4 1.385(5) ?
C3 H3 0.9300 ?
C4 C5 1.395(5) ?
C4 H4 0.9300 ?
C5 C6 1.375(5) ?
C5 H5 0.9300 ?
C6 C7 1.387(4) ?
C6 C8 1.519(5) ?
C7 C9 1.443(4) ?
C9 C10 1.377(4) ?
C13 C12 1.379(4) ?
C13 H13 0.9300 ?
C12 C11 1.384(4) ?
C12 H12 0.9300 ?
C11 C10 1.383(4) ?
C11 H11 0.9300 ?
C10 C8 1.521(4) ?
