What kind of interactions we may get moving from zwitter to “dritter” ions: C–O⋯Re(O4) and Re–O⋯Re(O4) anion⋯anion interactions make structural difference between l-histidinium perrhenate and pertechnetate
Novikov, Anton P.; Safonov, Alexey V.; German, Konstantin E.; Grigoriev, Mikhail S.; CrystEngComm 26 (2024) 61–69; doi:10.1039/D3CE01164J

data_7247923
_publ_section_title
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 What kind of interactions we may get moving from zwitter to
 &#x201C;dritter&#x201D; ions: C--O&#x22EF;Re(O4) and Re--O&#x22EF;Re(O4)
 anion&#x22EF;anion interactions make structural difference between
 l-histidinium perrhenate and pertechnetate
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              61
_journal_page_last               69
_journal_paper_doi               10.1039/D3CE01164J
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'O4 Tc, C6 H10 N3 O2'
_chemical_formula_sum            'C6 H10 N3 O6 Tc'
_chemical_formula_weight         319.08
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-03 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.147(4)
_cell_angle_beta                 87.966(4)
_cell_angle_gamma                62.592(4)
_cell_formula_units_Z            4
_cell_length_a                   9.9684(11)
_cell_length_b                   10.4769(12)
_cell_length_c                   11.0045(12)
_cell_measurement_reflns_used    2691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.586
_cell_measurement_theta_min      3.705
_cell_volume                     1019.6(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.1272
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18722
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         4.092
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0779 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.8461.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.811
_refine_diff_density_min         -2.043
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details
;
 Flack x determined using 2030 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9780
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0743
_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/[\s^2^(Fo^2^)+(0.0615P)^2^+8.9641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.652
_reflns_Friedel_fraction_full    0.712
_reflns_Friedel_fraction_max     0.649
_reflns_number_gt                7412
_reflns_number_total             9780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01164j2.cif
_cod_data_source_block           histc_lt_1_0m
_cod_database_code               7247923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93953
 0.06047
2. Uiso/Uaniso restraints and constraints
Uanis(N41) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.002
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(N31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C31) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(O45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3.a Ternary CH refined with riding coordinates:
 C42(H42A), C22(H22A), C32(H32A), C12(H12A)
3.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C43(H43A,H43B), C13(H13A,H13B), C23(H23A,H23B)
3.c Aromatic/amide H refined with riding coordinates:
 N33(H33), N32(H32), N12(H12), N22(H22), C26(H26), C46(H46), N23(H23),
 N42(H42), C16(H16), N13(H13), N43(H43), C36(H36), C45(H45), C25(H25), C15(H15),
  C35(H35)
3.d Idealised Me refined as rotating group:
 N31(H31A,H31B,H31C), N21(H21A,H21B,H21C), N11(H11A,H11B,H11C), N41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              98732
_olex2_submission_special_instructions 'No special instructions were received'