Exploring Second Coordination Sphere Effects in Flavodiiron Nitric Oxide Reductase Model Complexes
Bracken, Abigail J.; Dong, Hai Thanh; Lengel, Michael O.; Lehnert, Nicolai; Dalton Transactions  (2023) –; doi:10.1039/D3DT02828C

data_7714363
_publ_section_title
;
 Exploring Second Coordination Sphere Effects in Flavodiiron Nitric Oxide
 Reductase Model Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02828C
_journal_year                    2023
_chemical_formula_moiety
;
 2(C45 H59 Fe2 N8 O5), 6(C F3 O3 S), 2.55(C H4 O)
;
_chemical_formula_sum            'C98.5 H128 F18 Fe4 N16 O30.5 S6'
_chemical_formula_weight         2781.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual-space
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2023-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.770(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1428(5)
_cell_length_b                   11.31840(10)
_cell_length_c                   42.5686(5)
_cell_measurement_reflns_used    40190
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.2040
_cell_measurement_theta_min      2.2470
_cell_volume                     11938.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            181810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.860
_diffrn_reflns_theta_min         2.219
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    5.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       needle
_exptl_crystal_F_000             5748
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1678
_refine_ls_number_reflns         22253
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1678P)^2^+13.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18485
_reflns_number_total             22253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02828c2.cif
_cod_data_source_block           hd2128
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C98.50 H128 F18 Fe4 N16 O30.50 S6'
_cod_database_code               7714363
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              73918