#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:22:54 +0200 (Sat 05 de Jun de 2021) $
#$Revision: 266148 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/04/7060499.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_7060499
loop_
_publ_author_name
'Mikhailov, Artem A.'
'Komarov, Vladislav Yu.'
'Pishchur, Denis P.'
'Schaniel, Dominik'
'Kostin, Gennadiy A.'
_publ_section_title
;
 Nitrosyl linkage photoisomerization in heteroleptic fluoride ruthenium
 complexes derived from labile nitrate precursors
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8192
_journal_page_last               8202
_journal_paper_doi               10.1039/D1NJ01038G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety
'0.67(C5 H12 F N4 O2 Ru), 0.67(C5 H13 F N4 O2 Ru), 2(Cl O4)'
_chemical_formula_sum            'C6.67 H16.67 Cl2 F1.33 N5.33 O10.67 Ru1.33'
_chemical_formula_weight         573.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2021-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.730(4)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   18.6327(8)
_cell_length_b                   13.8821(5)
_cell_length_c                   10.4352(5)
_cell_measurement_reflns_used    10100
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.6500
_cell_measurement_theta_min      2.3620
_cell_volume                     2680.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4508
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00  10.00   1.00   25.00    --  -19.97 -57.00 -30.00  104
  2  ω    -53.00  50.00   1.00   25.00    --   20.91 -57.00-120.00  103
  3  ω    -53.00  50.00   1.00   25.00    --   20.91 -57.00   0.00  103
  4  ω    -53.00  50.00   1.00   25.00    --   20.91 -57.00-180.00  103
  5  ω    -94.00 -66.00   1.00   25.00    --  -19.97 -57.00  90.00   28
  6  ω    -94.00  10.00   1.00   25.00    --  -19.97 -57.00-150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0296255000
_diffrn_orient_matrix_UB_12      0.0258794000
_diffrn_orient_matrix_UB_13      0.0322166000
_diffrn_orient_matrix_UB_21      -0.0073589000
_diffrn_orient_matrix_UB_22      0.0388918000
_diffrn_orient_matrix_UB_23      -0.0436561000
_diffrn_orient_matrix_UB_31      -0.0231746000
_diffrn_orient_matrix_UB_32      0.0206908000
_diffrn_orient_matrix_UB_33      0.0417473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            44028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.915
_diffrn_reflns_theta_min         2.201
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.131
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.036
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         9455
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0395
_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)+(0.0262P)²+3.8829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6755
_reflns_number_total             9455
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj01038g2.cif
_cod_data_source_block           gs
_cod_depositor_comments
'Adding full bibliography for 7060496--7060499.cif.'
_cod_database_code               7060499
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 N4 O9 C10 H16 F1 Cl2'
_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_max   0.982
_shelx_estimated_absorpt_t_min   0.947
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O21-H21B
 0.85 with sigma of 0.02
3.a Rotating group:
 O21(H21A), O22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C52(H52), C11(H11), C12(H12), C51(H51), C41(H41), C21(H21),
 C42(H42), C32(H32), C22(H22D)
3.c Idealised Me refined as rotating group:
 N21(H21C,H21D,H21E), N22(H22A,H22B,H22C), N31(H31A,H31B,H31C), N32(H32A,H32B,
 H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.698
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru2 Ru 0.83124(2) 0.45274(2) 0.70635(2) 0.00874(6) Uani 1 1 d . . . . .
Ru1 Ru 0.65662(2) 0.44883(2) 0.28530(2) 0.00863(6) Uani 1 1 d . . . . .
Cl3 Cl 0.75255(4) 0.78111(5) 0.51286(7) 0.01187(13) Uani 1 1 d . . . . .
Cl5 Cl 0.59814(4) 0.11416(5) 0.33573(7) 0.01472(14) Uani 1 1 d . . . . .
Cl4 Cl 0.89694(4) 0.11131(5) 0.66438(7) 0.01451(14) Uani 1 1 d . . . . .
F12 F 0.86013(9) 0.55158(12) 0.59451(17) 0.0145(3) Uani 1 1 d . . . . .
F11 F 0.62225(9) 0.54604(12) 0.39216(18) 0.0156(4) Uani 1 1 d . . . . .
O21 O 0.67998(12) 0.37284(15) 0.4524(2) 0.0137(4) Uani 1 1 d D . . . .
H21A H 0.657193 0.318901 0.446961 0.021 Uiso 1 1 d GR . . . .
O22 O 0.80493(11) 0.37525(15) 0.5412(2) 0.0136(4) Uani 1 1 d . . . . .
H22 H 0.830040 0.323185 0.543963 0.020 Uiso 1 1 d GR . . . .
O35 O 0.59654(12) 0.20399(15) 0.4048(2) 0.0183(5) Uani 1 1 d . . . . .
O12 O 0.77908(12) 0.30597(16) 0.8680(2) 0.0175(5) Uani 1 1 d . . . . .
O11 O 0.71580(12) 0.30558(15) 0.1267(2) 0.0166(4) Uani 1 1 d . . . . .
O13 O 0.70783(13) 0.69931(16) 0.4740(2) 0.0220(5) Uani 1 1 d . . . . .
O34 O 0.89206(13) 0.19963(15) 0.5915(2) 0.0203(5) Uani 1 1 d . . . . .
N42 N 0.93511(12) 0.39669(17) 0.7151(2) 0.0102(4) Uani 1 1 d . . . . .
O43 O 0.82489(12) 0.76496(16) 0.4833(2) 0.0206(5) Uani 1 1 d . . . . .
N41 N 0.55245(13) 0.39070(16) 0.2725(2) 0.0103(5) Uani 1 1 d . . . . .
O23 O 0.75197(14) 0.7960(2) 0.6504(2) 0.0280(6) Uani 1 1 d . . . . .
O33 O 0.72357(13) 0.86616(16) 0.4467(3) 0.0250(5) Uani 1 1 d . . . . .
O14 O 0.84410(14) 0.04334(17) 0.6035(2) 0.0237(5) Uani 1 1 d . . . . .
O25 O 0.65632(14) 0.05484(17) 0.3967(2) 0.0256(6) Uani 1 1 d . . . . .
N21 N 0.75690(13) 0.52049(18) 0.3223(2) 0.0136(5) Uani 1 1 d . . . . .
H21C H 0.775835 0.529838 0.246755 0.016 Uiso 1 1 calc GR . . . .
H21D H 0.787801 0.484056 0.376222 0.016 Uiso 1 1 calc GR . . . .
H21E H 0.750256 0.578468 0.359879 0.016 Uiso 1 1 calc GR . . . .
N11 N 0.69082(12) 0.36280(17) 0.1879(2) 0.0108(5) Uani 1 1 d . . . . .
N12 N 0.80102(12) 0.36534(17) 0.8061(2) 0.0098(4) Uani 1 1 d . . . . .
N22 N 0.72975(13) 0.52199(18) 0.6767(3) 0.0145(5) Uani 1 1 d . . . . .
H22A H 0.733315 0.575877 0.628172 0.017 Uiso 1 1 calc GR . . . .
H22B H 0.715597 0.538664 0.754238 0.017 Uiso 1 1 calc GR . . . .
H22C H 0.696606 0.481284 0.634860 0.017 Uiso 1 1 calc GR . . . .
N31 N 0.62428(14) 0.54620(18) 0.1369(3) 0.0147(5) Uani 1 1 d . . . . .
H31A H 0.630798 0.519209 0.059627 0.018 Uiso 1 1 calc GR . . . .
H31B H 0.651202 0.600861 0.148580 0.018 Uiso 1 1 calc GR . . . .
H31C H 0.576748 0.560908 0.137849 0.018 Uiso 1 1 calc GR . . . .
O44 O 0.88100(17) 0.1295(2) 0.7929(2) 0.0397(8) Uani 1 1 d . . . . .
N32 N 0.86823(14) 0.54939(17) 0.8540(3) 0.0144(5) Uani 1 1 d . . . . .
H32A H 0.841910 0.604687 0.844568 0.017 Uiso 1 1 calc GR . . . .
H32B H 0.915650 0.563013 0.849644 0.017 Uiso 1 1 calc GR . . . .
H32C H 0.863167 0.522398 0.931929 0.017 Uiso 1 1 calc GR . . . .
O24 O 0.96750(14) 0.0722(2) 0.6629(4) 0.0466(9) Uani 1 1 d . . . . .
O45 O 0.6105(2) 0.1320(3) 0.2060(3) 0.0557(11) Uani 1 1 d . . . . .
C31 C 0.41453(16) 0.3144(2) 0.2685(3) 0.0159(6) Uani 1 1 d . . . . .
H31 H 0.367251 0.288487 0.266848 0.019 Uiso 1 1 calc R . . . .
C52 C 0.96685(15) 0.3509(2) 0.8201(3) 0.0140(6) Uani 1 1 d . . . . .
H52 H 0.940943 0.344383 0.892744 0.017 Uiso 1 1 calc R . . . .
C11 C 0.51512(16) 0.4013(2) 0.3750(3) 0.0128(5) Uani 1 1 d . . . . .
H11 H 0.536832 0.435010 0.448819 0.015 Uiso 1 1 calc R . . . .
C12 C 0.97125(16) 0.4049(2) 0.6110(3) 0.0139(6) Uani 1 1 d . . . . .
H12 H 0.948573 0.435937 0.535793 0.017 Uiso 1 1 calc R . . . .
C51 C 0.52165(16) 0.3418(2) 0.1687(3) 0.0134(5) Uani 1 1 d . . . . .
H51 H 0.547912 0.333929 0.096657 0.016 Uiso 1 1 calc R . . . .
O15 O 0.53181(15) 0.0656(2) 0.3447(4) 0.0670(13) Uani 1 1 d . . . . .
C41 C 0.45334(16) 0.3028(2) 0.1635(3) 0.0171(6) Uani 1 1 d . . . . .
H41 H 0.433025 0.268476 0.089266 0.021 Uiso 1 1 calc R . . . .
C21 C 0.44588(16) 0.3644(2) 0.3755(3) 0.0153(6) Uani 1 1 d . . . . .
H21 H 0.420378 0.373323 0.448257 0.018 Uiso 1 1 calc R . . . .
C42 C 1.03548(17) 0.3130(2) 0.8265(3) 0.0194(6) Uani 1 1 d . . . . .
H42 H 1.056466 0.280810 0.902161 0.023 Uiso 1 1 calc R . . . .
C32 C 1.07355(17) 0.3227(2) 0.7200(3) 0.0196(7) Uani 1 1 d . . . . .
H32 H 1.121202 0.297979 0.721966 0.023 Uiso 1 1 calc R . . . .
C22 C 1.04061(17) 0.3692(2) 0.6111(3) 0.0165(6) Uani 1 1 d . . . . .
H22D H 1.065409 0.376392 0.537114 0.020 Uiso 1 1 calc R . . . .
H21B H 0.7250(13) 0.368(4) 0.487(5) 0.075(19) Uiso 1 1 d 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'
Cl Cl 0.1484 0.1585 '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'
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'
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
_geom_angle_publ_flag
F12 Ru2 O22 85.41(8) . . ?
F12 Ru2 N42 88.17(8) . . ?
F12 Ru2 N22 84.00(8) . . ?
F12 Ru2 N32 84.14(9) . . ?
O22 Ru2 N42 88.27(9) . . ?
O22 Ru2 N22 89.65(9) . . ?
O22 Ru2 N32 169.29(9) . . ?
N42 Ru2 N22 172.04(9) . . ?
N42 Ru2 N32 89.04(10) . . ?
N12 Ru2 F12 177.33(9) . . ?
N12 Ru2 O22 94.33(10) . . ?
N12 Ru2 N42 94.47(10) . . ?
N12 Ru2 N22 93.34(10) . . ?
N12 Ru2 N32 96.21(11) . . ?
N32 Ru2 N22 91.60(10) . . ?
F11 Ru1 O21 85.35(8) . . ?
F11 Ru1 N41 86.44(8) . . ?
F11 Ru1 N21 84.86(9) . . ?
F11 Ru1 N31 83.59(9) . . ?
O21 Ru1 N41 87.64(9) . . ?
O21 Ru1 N21 89.53(9) . . ?
O21 Ru1 N31 168.92(9) . . ?
N41 Ru1 N21 171.03(9) . . ?
N11 Ru1 F11 177.88(9) . . ?
N11 Ru1 O21 95.08(10) . . ?
N11 Ru1 N41 95.66(10) . . ?
N11 Ru1 N21 93.07(10) . . ?
N11 Ru1 N31 96.00(11) . . ?
N31 Ru1 N41 90.99(10) . . ?
N31 Ru1 N21 90.16(10) . . ?
O13 Cl3 O23 108.65(15) . . ?
O13 Cl3 O33 109.88(15) . . ?
O43 Cl3 O13 110.12(14) . . ?
O43 Cl3 O23 110.51(15) . . ?
O43 Cl3 O33 109.52(14) . . ?
O33 Cl3 O23 108.13(16) . . ?
O35 Cl5 O25 109.28(15) . . ?
O45 Cl5 O35 109.91(18) . . ?
O45 Cl5 O25 108.72(16) . . ?
O15 Cl5 O35 107.95(15) . . ?
O15 Cl5 O25 108.3(2) . . ?
O15 Cl5 O45 112.7(3) . . ?
O34 Cl4 O14 108.91(15) . . ?
O44 Cl4 O34 109.74(17) . . ?
O44 Cl4 O14 108.65(15) . . ?
O24 Cl4 O34 108.66(15) . . ?
O24 Cl4 O14 109.04(17) . . ?
O24 Cl4 O44 111.8(2) . . ?
C52 N42 Ru2 122.14(19) . . ?
C52 N42 C12 118.9(3) . . ?
C12 N42 Ru2 118.9(2) . . ?
C11 N41 Ru1 117.8(2) . . ?
C51 N41 Ru1 123.38(19) . . ?
C51 N41 C11 118.8(3) . . ?
O11 N11 Ru1 177.4(2) . . ?
O12 N12 Ru2 177.1(2) . . ?
C21 C31 C41 118.9(3) . . ?
N42 C52 C42 122.6(3) . . ?
N41 C11 C21 121.8(3) . . ?
N42 C12 C22 121.6(3) . . ?
N41 C51 C41 122.2(3) . . ?
C51 C41 C31 119.1(3) . . ?
C31 C21 C11 119.1(3) . . ?
C52 C42 C32 118.7(3) . . ?
C22 C32 C42 118.8(3) . . ?
C12 C22 C32 119.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru2 F12 1.9188(16) . ?
Ru2 O22 2.042(2) . ?
Ru2 N42 2.078(2) . ?
Ru2 N12 1.735(2) . ?
Ru2 N22 2.112(2) . ?
Ru2 N32 2.098(3) . ?
Ru1 F11 1.9085(16) . ?
Ru1 O21 2.041(2) . ?
Ru1 N41 2.092(2) . ?
Ru1 N21 2.112(2) . ?
Ru1 N11 1.737(2) . ?
Ru1 N31 2.090(2) . ?
Cl3 O13 1.438(2) . ?
Cl3 O43 1.435(2) . ?
Cl3 O23 1.452(2) . ?
Cl3 O33 1.440(2) . ?
Cl5 O35 1.443(2) . ?
Cl5 O25 1.448(2) . ?
Cl5 O45 1.422(3) . ?
Cl5 O15 1.421(3) . ?
Cl4 O34 1.440(2) . ?
Cl4 O14 1.455(2) . ?
Cl4 O44 1.430(3) . ?
Cl4 O24 1.424(3) . ?
O12 N12 1.151(3) . ?
O11 N11 1.151(3) . ?
N42 C52 1.343(4) . ?
N42 C12 1.348(4) . ?
N41 C11 1.351(4) . ?
N41 C51 1.348(4) . ?
C31 C41 1.391(4) . ?
C31 C21 1.384(4) . ?
C52 C42 1.377(4) . ?
C11 C21 1.389(4) . ?
C12 C22 1.384(4) . ?
C51 C41 1.378(4) . ?
C42 C32 1.394(4) . ?
C32 C22 1.386(5) . ?
