Historical account of dinitrogen-bridged diiron complex synthesis using a commercial tripodal ligand
Smythe, Nathan C.; Mondal, Joydeb; Duque, Juan G.; Feller, Russell K.; Flores, Marco; Gordon, John C.; Henson, Neil J.; Paz-Pasternak, Moshe; Rein, Francisca N.; Scott, Brian L.; Taylor, R. Dean; Trovitch, Ryan J.; Chemical Communications 61 (2025) 9908–9911; doi:10.1039/D5CC02058A

data_7134646
_publ_section_title
;
 Historical account of dinitrogen-bridged diiron complex synthesis using a
 commercial tripodal ligand
;
_journal_issue                   54
_journal_name_full               'Chemical Communications'
_journal_page_first              9908
_journal_page_last               9911
_journal_paper_doi               10.1039/D5CC02058A
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C82 H78 Fe2 N2 P6'
_chemical_formula_weight         1388.98
_chemical_name_common            Mondal_1_262_2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2025-04-10 deposited with the CCDC.	2025-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.7264(5)
_cell_length_b                   15.2574(3)
_cell_length_c                   21.1376(4)
_cell_measurement_reflns_used    9652
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.2529
_cell_measurement_theta_min      2.2876
_cell_volume                     6931.3(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection
'Bruker Instrument Service (BIS) v8.5.0.15-rc12 (Bruker Nano, Inc., 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_publication_material  'APEX5 v2023.9-4 (Bruker AXS Inc., 2023)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            349913
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.95
_diffrn_source                   ' microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.493
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         12710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0448P)^2^+5.9205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10789
_reflns_number_total             12710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02058a2.cif
_cod_data_source_block           Mondal_1_262_2
_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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134646.cif.
;
_cod_database_code               7134646
_shelx_res_checksum              2861
_shelx_hkl_checksum              87210