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_7248236
_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         'C11 H15 Cl2 N4 O2 Tc'
_chemical_formula_sum            'C11 H15 Cl2 N4 O2 Tc'
_chemical_formula_weight         404.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 108.857(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.0605(6)
_cell_length_b                   33.630(3)
_cell_length_c                   12.0796(9)
_cell_measurement_reflns_used    3694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.723
_cell_measurement_theta_min      3.564
_cell_volume                     3098.7(4)
_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_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            54400
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         4.086
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.7396
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0741 before and 0.0680 after correction.
The Ratio of minimum to maximum transmission is 0.9298.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         9011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+2.6433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6048
_reflns_number_total             9011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00029c2.cif
_cod_data_source_block           mv14_lt_0m
_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            'C22 H30 Cl4 N8 O4 Tc2'
_cod_original_formula_weight         808.34
_cod_original_formula_moiety         '2(C11 H15 Cl2 N4 O2 Tc)'
_cod_original_formula_units_Z            4
_cod_database_code               7248236
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.831
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C9(H9A,H9B), C29(H29A,H29B)
1.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C3(H3), C8(H8), C6(H6), C21(H21), C7(H7), C22(H22), C5(H5),
 C26(H26), C25(H25), C23(H23), C4(H4), C24(H24), C28(H28), C27(H27)
1.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              13616
_olex2_submission_special_instructions 'No special instructions were received'