Highly malleable haem-binding site of the haemoprotein HasA permits stable accommodation of bulky tetraphenylporphycenes
Sakakibara, Erika; Shisaka, Yuma; Onoda, Hiroki; Koga, Daiki; Xu, Ning; Ono, Toshikazu; Hisaeda, Yoshio; Sugimoto, Hiroshi; Shiro, Yoshitsugu; Watanabe, Yoshihito; Shoji, Osami; RSC Advances 9 (2019) 18697–; doi:10.1039/C9RA02872B

data_7234981
_publ_section_title
;
 Highly malleable haem-binding site of the haemoprotein HasA permits
 stable accommodation of bulky tetraphenylporphycenes
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              18697
_journal_paper_doi               10.1039/C9RA02872B
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C88 H56 Fe2 N8 O'
_chemical_formula_sum            'C88 H56 Fe2 N8 O'
_chemical_formula_weight         1353.10
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-20
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2019-04-08 deposited with the CCDC.	2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9013(3)
_cell_length_b                   17.9013(3)
_cell_length_c                   42.9649(8)
_cell_measurement_reflns_used    7906
_cell_measurement_temperature    93
_cell_measurement_theta_max      28.9190
_cell_measurement_theta_min      2.5870
_cell_volume                     13768.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00 118.00   0.75   75.00    --   30.00  54.00-150.00  256
  2  \w    -74.00  27.25   0.75   75.00    --   30.00  54.00  30.00  135
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153013000
_diffrn_orient_matrix_UB_12      0.0346561000
_diffrn_orient_matrix_UB_13      0.0048420000
_diffrn_orient_matrix_UB_21      -0.0306595000
_diffrn_orient_matrix_UB_22      -0.0190603000
_diffrn_orient_matrix_UB_23      0.0068172000
_diffrn_orient_matrix_UB_31      0.0198752000
_diffrn_orient_matrix_UB_32      -0.0026470000
_diffrn_orient_matrix_UB_33      0.0142310000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0590
_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       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            35926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             5600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         7049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5243
_reflns_number_total             7049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02872b2.cif
_cod_data_source_block           xu017
_cod_original_cell_volume        13768.4(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7234981
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Fe Cl'
_chemical_oxdiff_usercomment     'Fe-PhPc (Cl anion Ch2Cl2 hexane)'
_diffrn_oxdiff_ac3_digest_frames
;
01b84de275002b8f4c809e416585e3f4e000391d57e
;
_diffrn_oxdiff_ac3_digest_hkl    01cfdcc26aa6282d2ab95a47ba7c02172d9f11
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C12(H12), C13(H13), C16(H16), C17(H17),
 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)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.476
_oxdiff_exptl_absorpt_empirical_full_min 0.724