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_7248237
_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         'C14 H21 Cl2 N4 O2 Tc'
_chemical_formula_sum            'C14 H21 Cl2 N4 O2 Tc'
_chemical_formula_weight         446.25
_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
_atom_sites_solution_primary     dual
_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                69.993(2)
_cell_angle_beta                 84.129(2)
_cell_angle_gamma                83.815(2)
_cell_formula_units_Z            4
_cell_length_a                   9.0399(5)
_cell_length_b                   14.1450(8)
_cell_length_c                   14.9860(8)
_cell_measurement_reflns_used    4539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.474
_cell_measurement_theta_min      2.608
_cell_volume                     1785.73(17)
_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 0.978
_diffrn_measured_fraction_theta_max 0.975
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24202
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         4.102
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0638 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.9018.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.807
_refine_diff_density_min         -2.129
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         8008
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+2.2487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6372
_reflns_number_total             8008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00029c2.cif
_cod_data_source_block           mv44_lt_2_0m
_cod_depositor_comments
'Adding full bibliography for 7248235--7248244.cif.'
_cod_database_code               7248237
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.663
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C11(H11A,H11B), C10(H10A,H10B), C30(H30A,
 H30B), C9(H9A,H9B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C23(H23), C21(H21), C4(H4), C26(H26), C2(H2), C3(H3),
 C5(H5), C28(H28), C6(H6), C1(H1), C27(H27), C25(H25), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              32296
_olex2_submission_special_instructions 'No special instructions were received'