Vibrational properties of heme-nitrosoalkane complexes in comparison with those of their HNO analogs, and reactivity studies towards nitric oxide and Lewis acids.
Harland, Jill B.; LaLonde, Ashley B.; Thomas, Diamond J.; Castella, Daniel G.; Kampf, Jeff W.; Zeller, Matthias; Alp, E. Ercan; Hu, Michael Y.; Zhao, Jiyong; Lehnert, Nicolai; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13906–13924; doi:10.1039/d4dt01632g

data_7716543
_publ_section_title
;
 Vibrational properties of heme-nitrosoalkane complexes in comparison with
 those of their HNO analogs, and reactivity studies towards nitric oxide
 and Lewis acids.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13906
_journal_page_last               13924
_journal_paper_doi               10.1039/d4dt01632g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C51 H43 Fe N5 O2'
_chemical_formula_sum            'C51 H43 Fe N6 O'
_chemical_formula_weight         811.76
_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
_audit_creation_date             2024-03-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.719(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4128(9)
_cell_length_b                   15.7751(10)
_cell_length_c                   18.9793(13)
_cell_measurement_reflns_used    56915
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      68.30
_cell_measurement_theta_min      2.30
_cell_volume                     4002.2(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      85.15
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            103181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.186
_diffrn_reflns_theta_min         4.335
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.394
_exptl_absorpt_correction_T_max  0.6853
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7302
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+8.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7093
_reflns_number_total             7302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01632g2.cif
_cod_data_source_block           abm3295
_cod_depositor_comments
'Adding full bibliography for 7716540--7716544.cif.'
_cod_database_code               7716543
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.496
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O2, O2A}
3. Rigid bond restraints
 O2, C48, C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C48A, C49A, C50A, C51A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O2 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
Uanis(C48A) \\sim Ueq, Uanis(C49A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) = Uanis(O2A)
5. Same fragment restrains
{O2, C51, C50, C49, C48} sigma for 1-2: 0.02, 1-3: 0.04
{O2A, C48A, C49A, C50A, C51A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O2, C48, C49, C50, C51}
6. Others
 Sof(O2A)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=Sof(H49D)=
 Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=1-FVAR(1)
 Sof(O2)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C45(H45)
7.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C48A(H48C,
 H48D), C49A(H49C,H49D), C50A(H50C,H50D), C51A(H51C,H51D)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C14(H14), C15(H15), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
7.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              86951
_shelx_hkl_checksum              73540
_olex2_submission_special_instructions 'No special instructions were received'