Structural, magnetic, redox and theoretical characterization of seven-coordinate first-row transition metal complexes with a macrocyclic ligand containing two benzimidazolyl N-pendant arms.
Drahoš, Bohuslav; Císařová, Ivana; Laguta, Oleksii; Santana, Vinicius T.; Neugebauer, Petr; Herchel, Radovan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4425–4440; doi:10.1039/d0dt00166j

data_7703741
_publ_section_title
;
 Structural, magnetic, redox and theoretical characterization of
 seven-coordinate first-row transition metal complexes with a macrocyclic
 ligand containing two benzimidazolyl N-pendant arms.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4425
_journal_page_last               4440
_journal_paper_doi               10.1039/d0dt00166j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C29 H33 N7 Ni O2, 2(Cl O4), 1.5(C H3 N O2)'
_chemical_formula_sum            'C30.5 H37.5 Cl2 N8.5 Ni O13'
_chemical_formula_weight         860.80
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-22 deposited with the CCDC.	2020-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                76.9370(10)
_cell_angle_beta                 76.3470(10)
_cell_angle_gamma                86.0280(10)
_cell_formula_units_Z            4
_cell_length_a                   13.8336(4)
_cell_length_b                   14.9837(4)
_cell_length_c                   18.6193(5)
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5223
_cell_measurement_theta_min      2.3059
_cell_volume                     3652.76(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2018.1.0.3'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NoniusKappa+Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61058
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         1.153
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.240
_refine_diff_density_max         1.473
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         16876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0689P)^2^+5.5450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13559
_reflns_number_total             16876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00166j2.cif
_cod_data_source_block           04
_cod_depositor_comments
;
Adding full bibliography for 7703738--7703741.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C29 H33 N7 Ni O2), 4(Cl O4), 3(C H3 N O2)'
_cod_original_formula_sum        'C61 H75 Cl4 N17 Ni2 O26'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1721.60
_cod_database_code               7703741
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.840
_shelx_res_checksum              33074
_shelx_fab_checksum              14248