The influence of the alkoxy substituent length on the crystal structures of Tc(v) complexes with pyrazine
Novikov, Anton P.; Volkov, Mikhail A.; CrystEngComm 26 (2024) 1747–1755; doi:10.1039/D4CE00029C

data_7248244
_publ_section_title
;
 The influence of the alkoxy substituent length on the crystal structures
 of Tc(v) complexes with pyrazine
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1747
_journal_page_last               1755
_journal_paper_doi               10.1039/D4CE00029C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C17 H27 Cl2 N4 O2 Tc'
_chemical_formula_sum            'C17 H27 Cl2 N4 O2 Tc'
_chemical_formula_weight         488.32
_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             2023-07-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-18 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                101.141(17)
_cell_angle_beta                 99.638(16)
_cell_angle_gamma                90.665(16)
_cell_formula_units_Z            4
_cell_length_a                   9.612(4)
_cell_length_b                   10.482(4)
_cell_length_c                   21.517(8)
_cell_measurement_reflns_used    302
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.262
_cell_measurement_theta_min      2.859
_cell_volume                     2094.9(14)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3360
_diffrn_reflns_av_unetI/netI     0.4121
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24079
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         4.133
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.9823
_exptl_absorpt_correction_T_min  0.8161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1064 before and 0.0877 after correction.
The Ratio of minimum to maximum transmission is 0.8308.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7336
_refine_ls_number_restraints     276
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.2912
_refine_ls_R_factor_gt           0.0925
_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^)+(0.0609P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.2352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2376
_reflns_number_total             7336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00029c2.cif
_cod_data_source_block           mv59
_cod_depositor_comments
;
Adding full bibliography for 7248235--7248244.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H54 Cl4 N8 O4 Tc2'
_cod_original_formula_weight         976.65
_cod_original_formula_moiety         '2(C17 H27 Cl2 N4 O2 Tc)'
_cod_original_formula_units_Z            2
_cod_database_code               7248244
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(N21)
\\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B)
2.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C37(H37A,H37B,H37C)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C1(H1), C25(H25),
 C26(H26), C27(H27), C28(H28), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              23710
_olex2_submission_special_instructions 'No special instructions were received'