#------------------------------------------------------------------------------
#$Date: 2019-11-23 12:47:21 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233340 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/87/4348787.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_4348787
loop_
_publ_author_name
'Fukushima, Takashi'
'Ghosh, Debashis'
'Kobayashi, Katsuaki'
'Ohtsu, Hideki'
'Kitagawa, Susumu'
'Tanaka, Koji'
_publ_section_title
;
 Four-Electron Reduction of a New Ruthenium Dicarbonyl Complex Having Two
 NAD Model Ligands through Decarboxylation in Water.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11613
_journal_page_last               11616
_journal_paper_doi               10.1021/acs.inorgchem.6b01619
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C38 H25 F12 N7 O2 P2 Ru'
_chemical_formula_weight         1002.66
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 115.263(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.036(4)
_cell_length_b                   13.849(3)
_cell_length_c                   16.632(4)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4662
_cell_measurement_theta_min      3.2388
_cell_volume                     3757.0(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-2011
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12056
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0441
_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)+(0.0519P)²+12.6000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2828
_reflns_number_total             3292
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01619_si_001.cif
_cod_data_source_block           pbn
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4348787
_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   0.959
_shelx_estimated_absorpt_t_max   0.959
_shelxl_version_number           2014-3
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
_atom_site_refinement_flags_occupancy
C1 C 0.5022(2) 0.3208(3) 0.3987(2) 0.0249(8) Uani 1 1 d . . .
C2 C 0.5313(2) 0.2784(3) 0.4840(2) 0.0289(8) Uani 1 1 d . . .
H2 H 0.5122 0.2166 0.4913 0.035 Uiso 1 1 calc R U .
C3 C 0.5864(2) 0.3260(3) 0.5549(2) 0.0286(8) Uani 1 1 d . . .
H3 H 0.6093 0.2958 0.6116 0.034 Uiso 1 1 calc R U .
N1 N 0.66274(18) 0.4686(2) 0.61741(19) 0.0291(7) Uani 1 1 d . . .
C4 C 0.7391(2) 0.6100(3) 0.6849(3) 0.0350(9) Uani 1 1 d . . .
H4 H 0.7633 0.5778 0.7406 0.042 Uiso 1 1 calc R U .
C5 C 0.7590(2) 0.7026(3) 0.6779(3) 0.0373(10) Uani 1 1 d . . .
H5 H 0.7983 0.7345 0.7288 0.045 Uiso 1 1 calc R U .
C6 C 0.7223(2) 0.7531(3) 0.5959(3) 0.0367(9) Uani 1 1 d . . .
H6 H 0.7369 0.8185 0.5930 0.044 Uiso 1 1 calc R U .
C7 C 0.6663(2) 0.7092(3) 0.5216(2) 0.0296(9) Uani 1 1 d . . .
H7 H 0.6414 0.7443 0.4675 0.036 Uiso 1 1 calc R U .
C8 C 0.5921(2) 0.5603(3) 0.4503(2) 0.0245(8) Uani 1 1 d . . .
H8 H 0.5672 0.5916 0.3943 0.029 Uiso 1 1 calc R U .
N2 N 0.52552(17) 0.4084(2) 0.38473(19) 0.0224(6) Uani 1 1 d . . .
C9 C 0.6102(2) 0.4213(3) 0.5449(2) 0.0262(8) Uani 1 1 d . . .
C10 C 0.5755(2) 0.4635(3) 0.4579(2) 0.0235(8) Uani 1 1 d . . .
C11 C 0.6815(2) 0.5604(3) 0.6081(2) 0.0266(8) Uani 1 1 d . . .
C12 C 0.6452(2) 0.6111(3) 0.5249(2) 0.0259(8) Uani 1 1 d . . .
C13 C 0.4422(2) 0.2701(3) 0.3194(2) 0.0271(8) Uani 1 1 d . . .
C14 C 0.4074(2) 0.1820(3) 0.3227(3) 0.0311(9) Uani 1 1 d . . .
H14 H 0.4253 0.1471 0.3769 0.037 Uiso 1 1 calc R U .
C15 C 0.3456(2) 0.1456(3) 0.2452(3) 0.0371(10) Uani 1 1 d . . .
H15 H 0.3212 0.0849 0.2456 0.045 Uiso 1 1 calc R U .
C16 C 0.3200(2) 0.1981(3) 0.1676(3) 0.0341(9) Uani 1 1 d . . .
H16 H 0.2762 0.1753 0.1148 0.041 Uiso 1 1 calc R U .
C17 C 0.3587(2) 0.2848(3) 0.1675(2) 0.0293(8) Uani 1 1 d . . .
H17 H 0.3417 0.3205 0.1137 0.035 Uiso 1 1 calc R U .
N3 N 0.41961(17) 0.3192(2) 0.24167(19) 0.0244(7) Uani 1 1 d . . .
C18 C 0.5806(2) 0.5294(3) 0.2634(2) 0.0243(8) Uani 1 1 d . . .
C19 C 0.5000 0.8239(6) 0.2500 0.092(4) Uani 1 2 d S T P
C20 C 0.5000 0.9284(6) 0.2500 0.127(6) Uani 1 2 d S T P
H20 H 0.4750 0.9519 0.1886 0.191 Uiso 0.5 1 calc R U P
H20A H 0.5565 0.9519 0.2799 0.191 Uiso 0.5 1 calc R U P
H20B H 0.4684 0.9519 0.2815 0.191 Uiso 0.5 1 calc R U P
F1 F 0.6102(2) 0.9386(2) 0.5108(3) 0.0811(11) Uani 1 1 d . . .
F2 F 0.69354(18) 1.1447(2) 0.5284(2) 0.0803(11) Uani 1 1 d . . .
F3 F 0.57722(15) 1.07848(18) 0.43507(16) 0.0487(7) Uani 1 1 d . . .
F4 F 0.7296(2) 1.0040(2) 0.6066(2) 0.0878(12) Uani 1 1 d . . .
F5 F 0.6112(3) 1.0794(3) 0.5814(2) 0.0963(14) Uani 1 1 d . . .
F6 F 0.6944(2) 1.0040(3) 0.4603(2) 0.0777(10) Uani 1 1 d . . .
Ru1 Ru 0.5000 0.43236(3) 0.2500 0.02193(15) Uani 1 2 d S T P
P1 P 0.65304(7) 1.04114(8) 0.52106(7) 0.0358(3) Uani 1 1 d . . .
O1 O 0.62764(16) 0.58672(19) 0.27093(17) 0.0327(6) Uani 1 1 d . . .
N4 N 0.5000 0.7426(6) 0.2500 0.130(4) Uani 1 2 d S T P
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
N2 C1 C2 122.8(3) . .
N2 C1 C13 116.1(3) . .
C2 C1 C13 121.0(3) . .
C3 C2 C1 119.7(4) . .
C2 C3 C9 120.0(3) . .
C11 N1 C9 118.4(3) . .
C5 C4 C11 119.9(4) . .
C4 C5 C6 121.2(4) . .
C7 C6 C5 120.9(4) . .
C6 C7 C12 120.0(4) . .
C10 C8 C12 120.0(3) . .
C1 N2 C10 118.6(3) . .
C1 N2 Ru1 112.6(2) . .
C10 N2 Ru1 127.5(2) . .
N1 C9 C3 118.8(3) . .
N1 C9 C10 122.9(4) . .
C3 C9 C10 118.2(3) . .
C8 C10 N2 122.1(3) . .
C8 C10 C9 117.8(3) . .
N2 C10 C9 120.1(3) . .
N1 C11 C4 118.4(3) . .
N1 C11 C12 122.7(3) . .
C4 C11 C12 118.9(4) . .
C8 C12 C7 123.0(3) . .
C8 C12 C11 117.9(4) . .
C7 C12 C11 119.1(3) . .
N3 C13 C14 121.5(3) . .
N3 C13 C1 114.7(3) . .
C14 C13 C1 123.7(3) . .
C13 C14 C15 118.7(4) . .
C16 C15 C14 119.5(4) . .
C15 C16 C17 119.3(4) . .
N3 C17 C16 121.3(4) . .
C17 N3 C13 119.5(3) . .
C17 N3 Ru1 126.7(3) . .
C13 N3 Ru1 113.1(2) . .
O1 C18 Ru1 179.6(4) . .
N4 C19 C20 180.0 . .
C18 Ru1 C18 91.2(2) . 2_655
C18 Ru1 N3 92.72(13) . 2_655
C18 Ru1 N3 175.46(13) 2_655 2_655
C18 Ru1 N3 175.46(13) . .
C18 Ru1 N3 92.72(13) 2_655 .
N3 Ru1 N3 83.41(16) 2_655 .
C18 Ru1 N2 100.07(13) . .
C18 Ru1 N2 92.55(12) 2_655 .
N3 Ru1 N2 88.92(11) 2_655 .
N3 Ru1 N2 77.56(11) . .
C18 Ru1 N2 92.55(12) . 2_655
C18 Ru1 N2 100.07(13) 2_655 2_655
N3 Ru1 N2 77.56(11) 2_655 2_655
N3 Ru1 N2 88.92(11) . 2_655
N2 Ru1 N2 161.95(16) . 2_655
F6 P1 F5 179.4(2) . .
F6 P1 F3 89.43(17) . .
F5 P1 F3 90.11(18) . .
F6 P1 F4 89.99(19) . .
F5 P1 F4 90.5(2) . .
F3 P1 F4 179.3(2) . .
F6 P1 F2 90.9(2) . .
F5 P1 F2 88.7(2) . .
F3 P1 F2 88.05(15) . .
F4 P1 F2 91.63(19) . .
F6 P1 F1 88.9(2) . .
F5 P1 F1 91.5(2) . .
F3 P1 F1 90.13(17) . .
F4 P1 F1 90.20(19) . .
F2 P1 F1 178.17(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.337(5) .
C1 C2 1.413(5) .
C1 C13 1.479(5) .
C2 C3 1.346(5) .
C3 C9 1.419(5) .
N1 C11 1.340(5) .
N1 C9 1.344(5) .
C4 C5 1.349(6) .
C4 C11 1.432(5) .
C5 C6 1.420(6) .
C6 C7 1.361(5) .
C7 C12 1.419(5) .
C8 C10 1.391(5) .
C8 C12 1.391(5) .
N2 C10 1.393(5) .
N2 Ru1 2.112(3) .
C9 C10 1.433(5) .
C11 C12 1.437(5) .
C13 N3 1.360(5) .
C13 C14 1.383(5) .
C14 C15 1.390(6) .
C15 C16 1.377(6) .
C16 C17 1.389(5) .
C17 N3 1.342(5) .
N3 Ru1 2.099(3) .
C18 O1 1.130(4) .
C18 Ru1 1.921(4) .
C19 N4 1.127(10) .
C19 C20 1.446(11) .
F1 P1 1.591(3) .
F2 P1 1.590(3) .
F3 P1 1.585(3) .
F4 P1 1.587(3) .
F5 P1 1.583(3) .
F6 P1 1.577(3) .
Ru1 C18 1.921(4) 2_655
Ru1 N3 2.099(3) 2_655
Ru1 N2 2.112(3) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N2 C1 C2 C3 -1.6(5)
C13 C1 C2 C3 179.5(3)
C1 C2 C3 C9 4.8(5)
C11 C4 C5 C6 1.5(6)
C4 C5 C6 C7 -0.6(6)
C5 C6 C7 C12 -1.3(6)
C2 C1 N2 C10 -5.2(5)
C13 C1 N2 C10 173.7(3)
C2 C1 N2 Ru1 162.8(3)
C13 C1 N2 Ru1 -18.3(4)
C11 N1 C9 C3 -176.5(3)
C11 N1 C9 C10 2.1(5)
C2 C3 C9 N1 177.3(3)
C2 C3 C9 C10 -1.3(5)
C12 C8 C10 N2 -177.3(3)
C12 C8 C10 C9 4.2(5)
C1 N2 C10 C8 -169.9(3)
Ru1 N2 C10 C8 24.2(5)
C1 N2 C10 C9 8.6(5)
Ru1 N2 C10 C9 -157.3(2)
N1 C9 C10 C8 -5.5(5)
C3 C9 C10 C8 173.1(3)
N1 C9 C10 N2 176.0(3)
C3 C9 C10 N2 -5.5(5)
C9 N1 C11 C4 -178.3(3)
C9 N1 C11 C12 2.6(5)
C5 C4 C11 N1 -179.7(4)
C5 C4 C11 C12 -0.5(5)
C10 C8 C12 C7 178.6(3)
C10 C8 C12 C11 0.1(5)
C6 C7 C12 C8 -176.3(4)
C6 C7 C12 C11 2.2(5)
N1 C11 C12 C8 -3.7(5)
C4 C11 C12 C8 177.3(3)
N1 C11 C12 C7 177.8(3)
C4 C11 C12 C7 -1.3(5)
N2 C1 C13 N3 1.2(5)
C2 C1 C13 N3 -179.9(3)
N2 C1 C13 C14 -175.4(3)
C2 C1 C13 C14 3.5(5)
N3 C13 C14 C15 -2.7(6)
C1 C13 C14 C15 173.6(3)
C13 C14 C15 C16 -0.8(6)
C14 C15 C16 C17 2.6(6)
C15 C16 C17 N3 -1.1(6)
C16 C17 N3 C13 -2.3(5)
C16 C17 N3 Ru1 167.2(3)
C14 C13 N3 C17 4.2(5)
C1 C13 N3 C17 -172.4(3)
C14 C13 N3 Ru1 -166.6(3)
C1 C13 N3 Ru1 16.8(4)
