Pressure-induced single-crystal-to-single-crystal nitrite ligand isomerisation accompanied by a piezochromic effect.
Potempa, Kinga; Paliwoda, Damian; Jarzembska, Katarzyna N.; Kamiński, Radosław; Krówczyński, Adam; Borowski, Patryk; Hanfland, Michael; Chemical communications (Cambridge, England) 60 (2024) 9194–9197; doi:10.1039/d4cc02898h

data_7133407
_publ_section_title
;
 Pressure-induced single-crystal-to-single-crystal nitrite ligand
 isomerisation accompanied by a piezochromic effect.
;
_journal_issue                   69
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9194
_journal_page_last               9197
_journal_paper_doi               10.1039/d4cc02898h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C15 H16 N6 Ni O4'
_chemical_formula_sum            'C15 H16 N6 Ni O4'
_chemical_formula_weight         403.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.60(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.295(3)
_cell_length_b                   9.5267(13)
_cell_length_c                   13.169(3)
_cell_measurement_reflns_used    420
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.2040
_cell_measurement_theta_min      2.6370
_cell_volume                     1561.3(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.474
_diffrn_measured_fraction_theta_max 0.268
_diffrn_measurement_device_type
'esperanto CrysAlisPro umported from ESRF ID15B beamline'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.40965
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.474
_diffrn_reflns_Laue_measured_fraction_max 0.268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1943
_diffrn_reflns_point_group_measured_fraction_full 0.375
_diffrn_reflns_point_group_measured_fraction_max 0.203
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         21.235
_diffrn_reflns_theta_min         1.987
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            piezochromic
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.35(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         1838
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+4.0959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.514
_reflns_Friedel_fraction_full    0.276
_reflns_Friedel_fraction_max     0.138
_reflns_number_gt                1584
_reflns_number_total             1838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02898h2.cif
_cod_data_source_block           Ni-diONO-16-I
_cod_depositor_comments
'Adding full bibliography for 7133389--7133407.cif.'
_cod_database_code               7133407
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C7A, C7B}
{C9A, C9B}
3. Restrained distances
 Ni1-O3A \\sim Ni1-O3B
 with sigma of 0.02
 O3A-N2A \\sim O3B-N2B
 with sigma of 0.02
 O4A-N2A \\sim O4B-N2B
 with sigma of 0.02
 Ni1-N2A \\sim Ni1-N2B
 with sigma of 0.04
 O3A-O4A \\sim O3B-O4B
 with sigma of 0.04
 Ni1-O1A \\sim Ni1-O1B
 with sigma of 0.02
 O1A-N1A \\sim O1B-N1B
 with sigma of 0.02
 O2A-N1A \\sim O2B-N1B
 with sigma of 0.02
 Ni1-N1A \\sim Ni1-N1B
 with sigma of 0.04
 O1A-O2A \\sim O1B-O2B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C8B \\sim C8A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O3A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
N2A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
O4A: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 2A
N6 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
O3A \\sim O3B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
N2B \\sim N2A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O4B \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O1A \\sim O1B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
N1B \\sim N1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O2B \\sim O2A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C8B) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C7A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C10) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O4B) \\sim Ueq, Uanis(N2B) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C7A) = Uanis(C7B)
Uanis(C9A) = Uanis(C9B)
5. Others
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=1-FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=FVAR(1)
 Sof(O1B)=Sof(O2B)=Sof(N1B)=1-FVAR(2)
 Sof(O1A)=Sof(O2A)=Sof(N1A)=FVAR(2)
 Sof(O3B)=Sof(O4B)=Sof(N2B)=1-FVAR(3)
 Sof(O3A)=Sof(O4A)=Sof(N2A)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C7B(H7BA,H7BB), C8B(H8BA,
 H8BB), C9B(H9BA,H9BB)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15),
 C6(H6), C10(H10)
6.c Fitted hexagon refined as free rotating group:
 N3(C1,C2,C3,C4,C5), N6(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              74208
_shelx_hkl_checksum              54742
_olex2_submission_special_instructions 'No special instructions were received'