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_1558805
_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         'C48 H64 Fe2 N4 S Si, 0.5(C5 H12)'
_chemical_formula_sum            'C50.5 H70 Fe2 N4 S Si'
_chemical_formula_weight         904.95
_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   mixed
_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                90
_cell_angle_beta                 94.457(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2840(3)
_cell_length_b                   14.0745(3)
_cell_length_c                   22.2861(4)
_cell_measurement_reflns_used    29297
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.5200
_cell_measurement_theta_min      3.0180
_cell_volume                     4779.57(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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 0.999
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         3.036
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       Block
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11850
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+3.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9521
_reflns_number_total             11850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03447a2.cif
_cod_data_source_block           007c-20026
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C50.50 H70 Fe2 N4 S Si'
_cod_database_code               1558805
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              3831