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_7133402
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-16
_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                90.205(14)
_cell_angle_beta                 105.14(2)
_cell_angle_gamma                87.019(15)
_cell_formula_units_Z            4
_cell_length_a                   12.208(3)
_cell_length_b                   9.1260(11)
_cell_length_c                   12.491(3)
_cell_measurement_reflns_used    316
_cell_measurement_temperature    293
_cell_measurement_theta_max      19.9020
_cell_measurement_theta_min      1.6040
_cell_volume                     1341.4(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.268
_diffrn_measured_fraction_theta_max 0.144
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_Laue_measured_fraction_full 0.268
_diffrn_reflns_Laue_measured_fraction_max 0.144
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3526
_diffrn_reflns_point_group_measured_fraction_full 0.268
_diffrn_reflns_point_group_measured_fraction_max 0.144
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         21.739
_diffrn_reflns_theta_min         1.587
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25719
_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    1.996
_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         0.819
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         2390
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0934
_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^)+(0.1618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1391
_reflns_number_total             2390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02898h2.cif
_cod_data_source_block           Ni-diONO-11-III
_cod_depositor_comments
'Adding full bibliography for 7133389--7133407.cif.'
_cod_database_code               7133402
_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. Uiso/Uaniso restraints and constraints
O8 \\sim N8 \\sim O7: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
O5 \\sim N7 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
O4 \\sim N2 \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
O2 \\sim N1 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(O4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N10) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C29) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N10) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N4) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C13) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B)
3.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), C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28),
 C29(H29), C30(H30), C21(H21), C25(H25)
3.c Fitted hexagon refined as free rotating group:
 N3(C1,C2,C3,C4,C5), N6(C11,C12,C13,C14,C15), N9(C16,C17,C18,C19,C20), N12(C26,
 C27,C28,C29,C30)
;
_shelx_res_checksum              77513
_shelx_hkl_checksum              12667
_olex2_submission_special_instructions 'No special instructions were received'