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_7133397
_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             2024-04-19
_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                90.02(3)
_cell_angle_beta                 106.67(3)
_cell_angle_gamma                105.24(3)
_cell_formula_units_Z            6
_cell_length_a                   19.686(4)
_cell_length_b                   9.307(2)
_cell_length_c                   12.765(3)
_cell_measurement_reflns_used    684
_cell_measurement_temperature    293
_cell_measurement_theta_max      19.6760
_cell_measurement_theta_min      2.2370
_cell_volume                     2154.4(10)
_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 0.272
_diffrn_measured_fraction_theta_max 0.147
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.272
_diffrn_reflns_Laue_measured_fraction_max 0.147
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5543
_diffrn_reflns_point_group_measured_fraction_full 0.272
_diffrn_reflns_point_group_measured_fraction_max 0.147
_diffrn_reflns_theta_full        14.229
_diffrn_reflns_theta_max         21.397
_diffrn_reflns_theta_min         1.562
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93067
_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    1.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     585
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0957P)^2^+1.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2649
_reflns_number_total             3762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02898h2.cif
_cod_data_source_block           Ni-diONO-07-II
_cod_depositor_comments
'Adding full bibliography for 7133389--7133407.cif.'
_cod_original_cell_volume        2154.4(9)
_cod_database_code               7133397
_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, All C(H,H,H,H) groups
2. Restrained distances
 O2A-N1A
 1.15 with sigma of 0.01
 N1A-O1B
 1.15 with sigma of 0.01
 O2B-Ni1
 2.15 with sigma of 0.02
 O1A-O2A
 2.07 with sigma of 0.01
 N1A-Ni1
 2.7 with sigma of 0.02
 Ni1-O2A \\sim Ni1-O2B
 with sigma of 0.02
 O2A-N1A \\sim O2B-N1B
 with sigma of 0.02
 O1A-N1A \\sim O1B-N1B
 with sigma of 0.02
 Ni1-N1A \\sim Ni1-N1B
 with sigma of 0.04
 O2A-O1A \\sim O2B-O1B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N6 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N3 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
N12 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N9 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim C16: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N15 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N18 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C23A \\sim C23B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O12 \\sim N14 \\sim O11: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O10 \\sim N13 \\sim O9: 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
N1A \\sim N1B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O1A \\sim O1B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O2B \\sim N1B \\sim O1B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O1B \\sim N1B \\sim O2B: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
O1A \\sim N1A \\sim O2A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
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(O3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O4) \\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(C21) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23A)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(N16) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O5) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O1A) \\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(O2A) \\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(N3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(O1B)=Sof(O2B)=Sof(N1B)=1-FVAR(2)
 Sof(O1A)=Sof(O2A)=Sof(N1A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C22(H22A,H22B), C22(H22C,H22D),
 C23A(H23A,H23B), C23B(H23C,H23D), C24(H24A,H24B), C24(H24C,H24D), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C1(H1), C2(H2), C3(H3), C4(H4),
 C10(H10), C6(H6), C16(H16), C17(H17), C18(H18), C19(H19), C27(H27), C28(H28),
 C29(H29), C30(H30), C21(H21), C25(H25), C34(H34), C33(H33), C32(H32), C31(H31),
  C45(H45), C44(H44), C43(H43), C42(H42), C36(H36), C40(H40)
5.c Fitted hexagon refined as free rotating group:
 N6(C11,C12,C13,C14,C15), N3(C1,C2,C3,C4,C5), N9(C16,C17,C18,C19,C20), N12(C26,
 C27,C28,C29,C30), N15(C35,C34,C33,C32,C31), N18(C45,C44,C43,C42,C41)
;
_shelx_res_checksum              46177
_shelx_hkl_checksum              27292
_olex2_submission_special_instructions 'No special instructions were received'