#------------------------------------------------------------------------------
#$Date: 2015-10-14 04:57:44 +0300 (Wed, 14 Oct 2015) $
#$Revision: 167923 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/02/2020212.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_2020212
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)3]'
_chemical_formula_moiety         'C14 H6 Cl2 N2 O4 Ru'
_chemical_formula_sum            'C14 H6 Cl2 N2 O4 Ru'
_chemical_formula_weight         438.18
_chemical_name_systematic
fac-Tricarbonyldichlorido(4,5-diazafluoren-9-one-κN)ruthenium(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_cell_angle_alpha                90.43(3)
_cell_angle_beta                 108.60(4)
_cell_angle_gamma                98.41(2)
_cell_formula_units_Z            2
_cell_length_a                   7.458(2)
_cell_length_b                   9.701(2)
_cell_length_c                   11.594(9)
_cell_measurement_reflns_used    2934
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.74
_cell_volume                     785.2(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.987
_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  0.0486
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7433
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.658
_diffrn_reflns_theta_min         1.856
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.597
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0372
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                2141
_reflns_number_total             2934
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ov3067sup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        785.1(7)
_cod_database_code               2020212
_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, -y, -z'
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 0.34512(5) 0.19385(3) 0.80951(3) 0.05637(13) Uani d 1
Cl Cl1 0.31437(16) -0.05628(10) 0.78187(11) 0.0812(4) Uani d 1
Cl Cl2 0.01300(14) 0.19209(12) 0.69578(13) 0.0944(4) Uani d 1
O O1 0.2193(5) 0.1340(3) 1.0283(3) 0.0996(9) Uani d 1
O O2 0.3520(4) 0.5013(3) 0.8646(2) 0.0701(8) Uani d 1
O O4 0.7583(4) 0.4634(3) 0.4104(3) 0.0928(10) Uani d 1
O O3 0.7628(4) 0.1844(3) 0.9465(3) 0.0816(9) Uani d 1
N N1 0.4091(4) 0.2135(3) 0.6401(3) 0.0517(8) Uani d 1
N N2 0.7099(4) 0.4535(3) 0.8075(3) 0.0539(8) Uani d 1
C C1 0.2690(8) 0.1590(5) 0.9463(5) 0.0996(9) Uani d 1
C C2 0.3567(5) 0.3899(4) 0.8389(3) 0.0543(10) Uani d 1
C C14 0.5432(5) 0.3041(4) 0.6140(3) 0.0472(9) Uani d 1
C C13 0.6820(5) 0.4209(4) 0.6922(4) 0.0460(9) Uani d 1
C C9 0.7831(5) 0.4932(4) 0.6231(4) 0.0558(10) Uani d 1
C C8 0.7136(6) 0.4259(5) 0.4978(4) 0.0647(12) Uani d 1
C C7 0.5671(6) 0.3054(4) 0.5003(4) 0.0552(10) Uani d 1
C C6 0.4577(7) 0.2099(5) 0.4087(4) 0.0749(13) Uani d 1
H H6 0.4751 0.2088 0.3328 0.090 Uiso calc 1
C C5 0.3210(7) 0.1158(5) 0.4337(4) 0.0775(14) Uani d 1
H H5 0.2432 0.0489 0.3740 0.093 Uiso calc 1
C C4 0.2986(6) 0.1201(4) 0.5465(4) 0.0706(12) Uani d 1
H H4 0.2029 0.0560 0.5602 0.085 Uiso calc 1
C C10 0.9183(6) 0.6085(4) 0.6741(5) 0.0684(12) Uani d 1
H H10 0.9866 0.6593 0.6297 0.082 Uiso calc 1
C C11 0.9465(6) 0.6442(4) 0.7941(5) 0.0739(13) Uani d 1
H H11 1.0349 0.7218 0.8331 0.089 Uiso calc 1
C C12 0.8448(6) 0.5657(4) 0.8559(4) 0.0644(11) Uani d 1
H H12 0.8703 0.5913 0.9377 0.077 Uiso calc 1
C C3 0.6052(7) 0.1911(4) 0.8956(4) 0.0611(11) 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
C1 Ru1 C3 93.5(2) y
C1 Ru1 C2 89.90(18) y
C3 Ru1 C2 95.34(16) y
C1 Ru1 N1 173.34(18) y
C3 Ru1 N1 90.43(15) y
C2 Ru1 N1 95.11(13) y
C1 Ru1 Cl2 87.35(18) y
C3 Ru1 Cl2 178.40(13) y
C2 Ru1 Cl2 86.04(12) y
N1 Ru1 Cl2 88.62(10) y
C1 Ru1 Cl1 85.99(15) y
C3 Ru1 Cl1 86.50(12) y
C2 Ru1 Cl1 175.60(11) y
N1 Ru1 Cl1 88.86(9) y
Cl2 Ru1 Cl1 92.18(5) y
C14 N1 C4 115.2(3) ?
C14 N1 Ru1 129.1(3) ?
C4 N1 Ru1 115.7(3) ?
C13 N2 C12 114.9(3) ?
O1 C1 Ru1 177.9(5) ?
O2 C2 Ru1 172.3(3) ?
N1 C14 C7 122.9(4) ?
N1 C14 C13 129.2(3) ?
C7 C14 C13 107.9(4) ?
N2 C13 C9 123.9(4) ?
N2 C13 C14 127.4(3) ?
C9 C13 C14 108.7(3) ?
C10 C9 C13 120.1(4) ?
C10 C9 C8 131.2(4) ?
C13 C9 C8 108.6(4) ?
O4 C8 C7 126.6(4) ?
O4 C8 C9 128.1(4) ?
C7 C8 C9 105.2(4) ?
C6 C7 C14 121.1(4) ?
C6 C7 C8 129.3(4) ?
C14 C7 C8 109.5(4) ?
C7 C6 C5 117.0(4) ?
C7 C6 H6 121.5 ?
C5 C6 H6 121.5 ?
C6 C5 C4 120.2(4) ?
C6 C5 H5 119.9 ?
C4 C5 H5 119.9 ?
N1 C4 C5 123.6(4) ?
N1 C4 H4 118.2 ?
C5 C4 H4 118.2 ?
C11 C10 C9 116.3(4) ?
C11 C10 H10 121.9 ?
C9 C10 H10 121.9 ?
C12 C11 C10 119.8(4) ?
C12 C11 H11 120.1 ?
C10 C11 H11 120.1 ?
N2 C12 C11 125.0(4) ?
N2 C12 H12 117.5 ?
C11 C12 H12 117.5 ?
O3 C3 Ru1 177.4(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 C1 1.865(5) y
Ru1 C3 1.882(5) y
Ru1 C2 1.914(4) y
Ru1 N1 2.168(3) y
Ru1 Cl2 2.4037(16) y
Ru1 Cl1 2.4128(12) y
O1 C1 1.141(5) ?
O2 C2 1.128(4) ?
O4 C8 1.206(4) ?
O3 C3 1.146(4) ?
N1 C14 1.344(4) ?
N1 C4 1.369(4) ?
N2 C13 1.314(4) ?
N2 C12 1.350(4) ?
C14 C7 1.385(5) ?
C14 C13 1.490(5) ?
C13 C9 1.394(5) ?
C9 C10 1.377(5) ?
C9 C8 1.488(5) ?
C8 C7 1.486(5) ?
C7 C6 1.365(5) ?
C6 C5 1.370(6) ?
C6 H6 0.9300 ?
C5 C4 1.372(5) ?
C5 H5 0.9300 ?
C4 H4 0.9300 ?
C10 C11 1.373(5) ?
C10 H10 0.9300 ?
C11 C12 1.362(5) ?
C11 H11 0.9300 ?
C12 H12 0.9300 ?

_cod_database_fobs_code 2020212
