The influences of carbon donor ligands on biomimetic multi-iron complexes for N2 reduction
Nagelski, Alexandra L.; Fataftah, Majed S.; Bollmeyer, Melissa M.; McWilliams, Sean F.; MacMillan, Samantha N.; Mercado, Brandon Q.; Lancaster, Kyle M.; Holland, Patrick L.; Chemical Science  (2020) –; doi:10.1039/D0SC03447A

data_1558804
_publ_section_title
;
 The influences of carbon donor ligands on biomimetic multi-iron complexes
 for N2 reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03447A
_journal_year                    2020
_chemical_formula_moiety
;
C26 H38 Fe N2 Si, 0.69(C4 H8 O), 0.31(C4 H10 O), 0.5(C4 H8 O), C12 H24 O K
;
_chemical_formula_sum            'C44 H74.63 Fe K N2 O7.5 Si'
_chemical_formula_weight         874.72
_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     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                73.777(2)
_cell_angle_beta                 85.650(3)
_cell_angle_gamma                86.169(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7212(4)
_cell_length_b                   13.5703(4)
_cell_length_c                   14.5849(5)
_cell_measurement_reflns_used    16989
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.6410
_cell_measurement_theta_min      3.0680
_cell_volume                     2407.84(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Dectris Pilatus 3R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.726
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       Block
_exptl_crystal_F_000             943
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9163
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0344P)^2^+2.6514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8132
_reflns_number_total             9163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03447a2.cif
_cod_data_source_block           007c-19063
_cod_original_formula_sum        'C44 H74.63 Fe K N2 O7.50 Si'
_cod_database_code               1558804
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.920
_shelx_res_checksum              88821