#------------------------------------------------------------------------------
#$Date: 2025-08-04 09:03:09 +0200 (Mon 04 de Aug de 2025) $
#$Revision: 301442 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/63/7056380.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_7056380
loop_
_publ_author_name
'Amabilino, Silvia'
'Tasse, Marine'
'Lacroix, Pascal G.'
'Mallet-Ladeira, Sonia'
'Pimienta, Véronique'
'Akl, Joëlle'
'Sasaki, Isabelle'
'Malfant, Isabelle'
_publ_section_title
;
 Photorelease of nitric oxide (NO) on ruthenium nitrosyl complexes with
 phenyl substituted terpyridines
;
_journal_issue                   15
_journal_name_full               'New J. Chem.'
_journal_page_first              7371
_journal_page_last               7383
_journal_paper_doi               10.1039/C7NJ00866J
_journal_volume                  41
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H14 Br Cl2 N4 O Ru, F6 P'
_chemical_formula_sum            'C21 H14 Br Cl2 F6 N4 O P Ru'
_chemical_formula_weight         735.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_update_record
;
2017-03-10 deposited with the CCDC.
2017-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8897(9)
_cell_length_b                   17.2969(13)
_cell_length_c                   13.3346(10)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.27
_cell_measurement_wavelength     0.71073
_cell_volume                     2422.0(3)
_computing_cell_refinement       'APEX2 and SAINT'
_computing_data_collection       APEX2
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker Kappa APEX II Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            50815
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.655
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.636
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0348P)²+5.2349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                4154
_reflns_number_total             5140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj00866j2.cif
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7056380
loop_
_symmetry_equiv_pos_as_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_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5000(4) 0.4240(2) 0.8088(3) 0.0244(8) Uani 1 1 d . . .
H1 H 0.5421 0.4337 0.8797 0.029 Uiso 1 1 calc R . .
C2 C 0.4789(4) 0.3488(2) 0.7747(3) 0.0262(9) Uani 1 1 d . . .
H2 H 0.505 0.307 0.8218 0.031 Uiso 1 1 calc R . .
C3 C 0.4198(4) 0.3348(2) 0.6717(3) 0.0252(8) Uani 1 1 d . . .
H3 H 0.4048 0.2831 0.6475 0.03 Uiso 1 1 calc R . .
C4 C 0.3818(4) 0.3959(2) 0.6031(3) 0.0206(8) Uani 1 1 d . . .
H4 H 0.3416 0.3867 0.5317 0.025 Uiso 1 1 calc R . .
C5 C 0.4038(3) 0.4707(2) 0.6412(3) 0.0183(7) Uani 1 1 d . . .
C6 C 0.3634(3) 0.54069(19) 0.5776(3) 0.0165(7) Uani 1 1 d . . .
C7 C 0.3214(3) 0.54455(19) 0.4705(3) 0.0171(7) Uani 1 1 d . . .
H7 H 0.3153 0.4989 0.4299 0.02 Uiso 1 1 calc R . .
C8 C 0.2876(3) 0.61664(19) 0.4216(3) 0.0165(7) Uani 1 1 d . . .
C9 C 0.3008(3) 0.6828(2) 0.4843(3) 0.0169(7) Uani 1 1 d . . .
H9 H 0.2788 0.7321 0.4533 0.02 Uiso 1 1 calc R . .
C10 C 0.3460(3) 0.67633(19) 0.5914(3) 0.0160(7) Uani 1 1 d . . .
C11 C 0.3710(3) 0.7397(2) 0.6679(3) 0.0176(7) Uani 1 1 d . . .
C12 C 0.3389(4) 0.8154(2) 0.6427(3) 0.0221(8) Uani 1 1 d . . .
H12 H 0.2983 0.8295 0.5729 0.026 Uiso 1 1 calc R . .
C13 C 0.3664(4) 0.8713(2) 0.7207(3) 0.0256(8) Uani 1 1 d . . .
H13 H 0.344 0.9238 0.7047 0.031 Uiso 1 1 calc R . .
C14 C 0.4265(4) 0.8498(2) 0.8210(3) 0.0257(8) Uani 1 1 d . . .
H14 H 0.446 0.8872 0.8751 0.031 Uiso 1 1 calc R . .
C15 C 0.4580(4) 0.7730(2) 0.8421(3) 0.0225(8) Uani 1 1 d . . .
H15 H 0.4998 0.7581 0.9113 0.027 Uiso 1 1 calc R . .
C16 C 0.2354(4) 0.6215(2) 0.3079(3) 0.0185(7) Uani 1 1 d . . .
C17 C 0.1799(4) 0.5568(2) 0.2508(3) 0.0214(8) Uani 1 1 d . . .
H17 H 0.1816 0.5085 0.285 0.026 Uiso 1 1 calc R . .
C18 C 0.1226(4) 0.5618(2) 0.1449(3) 0.0262(9) Uani 1 1 d . . .
H18 H 0.0861 0.5175 0.1064 0.031 Uiso 1 1 calc R . .
C19 C 0.1196(4) 0.6325(2) 0.0967(3) 0.0235(8) Uani 1 1 d . . .
C20 C 0.1777(4) 0.6973(2) 0.1496(3) 0.0245(8) Uani 1 1 d . . .
H20 H 0.1782 0.7449 0.1142 0.029 Uiso 1 1 calc R . .
C21 C 0.2348(4) 0.6913(2) 0.2550(3) 0.0218(8) Uani 1 1 d . . .
H21 H 0.2745 0.7355 0.2922 0.026 Uiso 1 1 calc R . .
Br1 Br 0.02724(4) 0.64194(2) -0.04571(3) 0.03048(12) Uani 1 1 d . . .
Cl1 Cl 0.59370(10) 0.59607(6) 0.95837(7) 0.0326(2) Uani 1 1 d . . .
Cl2 Cl 0.64419(9) 0.61435(5) 0.72711(8) 0.0252(2) Uani 1 1 d . . .
P1 P 1.00798(9) 0.62209(6) 0.63749(7) 0.0218(2) Uani 1 1 d U . .
F1 F 1.0820(9) 0.5958(5) 0.5588(7) 0.0354(17) Uani 0.670(17) 1 d PU A 1
F2 F 1.0538(8) 0.5501(4) 0.7104(6) 0.0458(18) Uani 0.670(17) 1 d PU A 1
F3 F 0.9310(6) 0.6545(6) 0.7199(4) 0.0364(15) Uani 0.670(17) 1 d PU A 1
F4 F 0.9585(10) 0.6987(6) 0.5680(7) 0.0345(18) Uani 0.670(17) 1 d PU A 1
F5 F 0.8828(10) 0.5791(6) 0.5756(9) 0.0316(18) Uani 0.670(17) 1 d PU A 1
F6 F 1.130(2) 0.6703(16) 0.7083(14) 0.028(2) Uani 0.670(17) 1 d PU A 1
F1' F 1.081(2) 0.6213(10) 0.5422(14) 0.034(3) Uani 0.330(17) 1 d PU A 2
F2' F 1.0959(16) 0.5448(8) 0.6800(12) 0.042(3) Uani 0.330(17) 1 d PU A 2
F3' F 0.9441(14) 0.6174(11) 0.7232(10) 0.042(3) Uani 0.330(17) 1 d PU A 2
F4' F 0.9288(19) 0.6916(14) 0.5847(16) 0.038(3) Uani 0.330(17) 1 d PU A 2
F5' F 0.905(2) 0.5601(11) 0.5653(19) 0.028(3) Uani 0.330(17) 1 d PU A 2
F6' F 1.120(5) 0.675(3) 0.692(3) 0.025(3) Uani 0.330(17) 1 d PU A 2
N1 N 0.3327(3) 0.58419(18) 0.8389(2) 0.0236(7) Uani 1 1 d . . .
N2 N 0.4624(3) 0.48397(17) 0.7437(2) 0.0197(6) Uani 1 1 d . . .
N3 N 0.3723(3) 0.60581(16) 0.6340(2) 0.0153(6) Uani 1 1 d . . .
N4 N 0.4312(3) 0.71896(17) 0.7675(2) 0.0186(6) Uani 1 1 d . . .
O1 O 0.2639(3) 0.5688(2) 0.8862(2) 0.0374(7) Uani 1 1 d . . .
Ru1 Ru 0.46111(3) 0.599943(16) 0.78413(2) 0.01724(9) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 0.006 '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
N2 C1 C2 121.3(4)
N2 C1 H1 119.3
C2 C1 H1 119.3
C3 C2 C1 119.3(3)
C3 C2 H2 120.4
C1 C2 H2 120.4
C2 C3 C4 120.3(3)
C2 C3 H3 119.9
C4 C3 H3 119.9
C5 C4 C3 118.4(3)
C5 C4 H4 120.8
C3 C4 H4 120.8
N2 C5 C4 120.9(3)
N2 C5 C6 115.2(3)
C4 C5 C6 123.9(3)
N3 C6 C7 119.6(3)
N3 C6 C5 113.6(3)
C7 C6 C5 126.9(3)
C6 C7 C8 119.7(3)
C6 C7 H7 120.2
C8 C7 H7 120.2
C9 C8 C7 118.3(3)
C9 C8 C16 121.1(3)
C7 C8 C16 120.5(3)
C10 C9 C8 120.0(3)
C10 C9 H9 120
C8 C9 H9 120
N3 C10 C9 119.1(3)
N3 C10 C11 113.8(3)
C9 C10 C11 127.1(3)
N4 C11 C12 120.9(3)
N4 C11 C10 115.6(3)
C12 C11 C10 123.5(3)
C11 C12 C13 119.3(3)
C11 C12 H12 120.4
C13 C12 H12 120.4
C14 C13 C12 119.4(4)
C14 C13 H13 120.3
C12 C13 H13 120.3
C13 C14 C15 119.1(3)
C13 C14 H14 120.5
C15 C14 H14 120.5
N4 C15 C14 121.7(3)
N4 C15 H15 119.1
C14 C15 H15 119.1
C21 C16 C17 118.2(3)
C21 C16 C8 121.2(3)
C17 C16 C8 120.6(3)
C18 C17 C16 121.1(3)
C18 C17 H17 119.4
C16 C17 H17 119.4
C19 C18 C17 118.6(3)
C19 C18 H18 120.7
C17 C18 H18 120.7
C18 C19 C20 122.0(3)
C18 C19 Br1 118.8(3)
C20 C19 Br1 119.2(3)
C21 C20 C19 118.7(3)
C21 C20 H20 120.7
C19 C20 H20 120.7
C20 C21 C16 121.2(3)
C20 C21 H21 119.4
C16 C21 H21 119.4
F3' P1 F4' 94.3(8)
F3' P1 F1 159.3(6)
F4' P1 F1 104.4(7)
F3' P1 F6' 98(2)
F4' P1 F6' 91.6(19)
F1 P1 F6' 90(2)
F3' P1 F2 67.7(6)
F4' P1 F2 161.3(6)
F1 P1 F2 92.8(3)
F6' P1 F2 95.6(17)
F3' P1 F5 82.1(6)
F4' P1 F5 80.0(9)
F1 P1 F5 92.3(5)
F6' P1 F5 171.6(18)
F2 P1 F5 92.2(5)
F3' P1 F4 109.3(7)
F1 P1 F4 90.4(4)
F6' P1 F4 83.3(17)
F2 P1 F4 176.7(4)
F5 P1 F4 88.6(5)
F3' P1 F6 93.4(10)
F4' P1 F6 97.9(12)
F1 P1 F6 92.9(10)
F2 P1 F6 88.3(8)
F5 P1 F6 174.8(11)
F4 P1 F6 90.6(9)
F4' P1 F3 73.5(7)
F1 P1 F3 177.1(3)
F6' P1 F3 88(2)
F2 P1 F3 89.5(3)
F5 P1 F3 89.3(4)
F4 P1 F3 87.2(4)
F6 P1 F3 85.5(10)
F3' P1 F2' 92.2(6)
F4' P1 F2' 172.9(9)
F1 P1 F2' 68.8(5)
F6' P1 F2' 90.3(19)
F5 P1 F2' 98.1(6)
F4 P1 F2' 158.2(6)
F6 P1 F2' 84.5(10)
F3 P1 F2' 113.4(5)
F3' P1 F5' 91.6(9)
F4' P1 F5' 91.6(11)
F1 P1 F5' 79.2(8)
F6' P1 F5' 169(2)
F2 P1 F5' 84.5(8)
F4 P1 F5' 97.1(8)
F6 P1 F5' 168.9(11)
F3 P1 F5' 102.7(7)
F2' P1 F5' 85.4(8)
F3' P1 F1' 176.4(7)
F4' P1 F1' 88.8(8)
F6' P1 F1' 83(2)
F2 P1 F1' 109.0(6)
F5 P1 F1' 96.7(8)
F4 P1 F1' 74.0(6)
F6 P1 F1' 88.0(12)
F3 P1 F1' 160.1(5)
F2' P1 F1' 84.6(7)
F5' P1 F1' 86.5(10)
O1 N1 Ru1 169.4(3)
C1 N2 C5 119.8(3)
C1 N2 Ru1 126.8(3)
C5 N2 Ru1 112.9(2)
C6 N3 C10 123.3(3)
C6 N3 Ru1 117.8(2)
C10 N3 Ru1 117.8(2)
C15 N4 C11 119.6(3)
C15 N4 Ru1 127.7(2)
C11 N4 Ru1 112.6(2)
N1 Ru1 N3 101.42(13)
N1 Ru1 N2 91.06(13)
N3 Ru1 N2 79.77(11)
N1 Ru1 N4 94.47(13)
N3 Ru1 N4 79.71(11)
N2 Ru1 N4 159.42(11)
N1 Ru1 Cl2 173.99(10)
N3 Ru1 Cl2 84.00(9)
N2 Ru1 Cl2 87.34(9)
N4 Ru1 Cl2 89.02(9)
N1 Ru1 Cl1 86.24(10)
N3 Ru1 Cl1 172.34(9)
N2 Ru1 Cl1 100.45(9)
N4 Ru1 Cl1 99.68(8)
Cl2 Ru1 Cl1 88.36(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N2 1.345(5)
C1 C2 1.377(5)
C1 H1 0.95
C2 C3 1.375(6)
C2 H2 0.95
C3 C4 1.388(5)
C3 H3 0.95
C4 C5 1.387(5)
C4 H4 0.95
C5 N2 1.367(4)
C5 C6 1.477(5)
C6 N3 1.343(4)
C6 C7 1.382(5)
C7 C8 1.410(5)
C7 H7 0.95
C8 C9 1.402(5)
C8 C16 1.474(5)
C9 C10 1.387(5)
C9 H9 0.95
C10 N3 1.344(4)
C10 C11 1.472(5)
C11 N4 1.364(4)
C11 C12 1.374(5)
C12 C13 1.393(5)
C12 H12 0.95
C13 C14 1.376(5)
C13 H13 0.95
C14 C15 1.383(5)
C14 H14 0.95
C15 N4 1.339(4)
C15 H15 0.95
C16 C21 1.397(5)
C16 C17 1.399(5)
C17 C18 1.387(5)
C17 H17 0.95
C18 C19 1.378(5)
C18 H18 0.95
C19 C20 1.384(5)
C19 Br1 1.906(4)
C20 C21 1.382(5)
C20 H20 0.95
C21 H21 0.95
Cl1 Ru1 2.3898(10)
Cl2 Ru1 2.3276(10)
P1 F3' 1.489(14)
P1 F4' 1.54(2)
P1 F1 1.550(9)
P1 F6' 1.55(5)
P1 F2 1.577(7)
P1 F5 1.580(11)
P1 F4 1.625(10)
P1 F6 1.64(2)
P1 F3 1.647(6)
P1 F2' 1.654(14)
P1 F5' 1.66(2)
P1 F1' 1.67(2)
N1 O1 1.132(4)
N1 Ru1 1.761(3)
N2 Ru1 2.078(3)
N3 Ru1 1.982(3)
N4 Ru1 2.087(3)
