Late first-row transition metal complexes of a 17-membered piperazine-based macrocyclic ligand: structures and magnetism.
Zahradníková, Eva; Herchel, Radovan; Šalitroš, Ivan; Císařová, Ivana; Drahoš, Bohuslav; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9057–9069; doi:10.1039/d0dt01392g

data_7704534
_publ_section_title
;
 Late first-row transition metal complexes of a 17-membered
 piperazine-based macrocyclic ligand: structures and magnetism.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9057
_journal_page_last               9069
_journal_paper_doi               10.1039/d0dt01392g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C19 H32 Fe N6,2(ClO4),0.5(C2H3N)'
_chemical_formula_sum            'C20 H33.5 Cl2 Fe N6.5 O8'
_chemical_formula_weight         619.78
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-04-15 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7424(4)
_cell_length_b                   11.1169(3)
_cell_length_c                   34.3592(10)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    187(2)
_cell_measurement_theta_max      31.0455
_cell_measurement_theta_min      2.1837
_cell_volume                     5232.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2019.1.0.1'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      187(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD with Bruker APEXII detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33592
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.189
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.485
_exptl_crystal_size_min          0.372
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         9179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+9.9718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8235
_reflns_number_total             9179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01392g2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7704533--7704535.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     '2(C19 H32 Fe N6),4(ClO4),C2H3N'
_cod_original_formula_sum        'C40 H67 Cl4 Fe2 N13 O16'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1239.56
_cod_database_code               7704534
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.642
_shelx_estimated_absorpt_t_max   0.746
_shelx_res_checksum              9330