Functional characterization of the halogenase SpmH and discovery of new deschloro-tryptophan dimers.
Liu, Zhiwen; Ma, Liang; Zhang, Liping; Zhang, Wenjun; Zhu, Yiguang; Chen, Yuchan; Zhang, Weimin; Zhang, Changsheng; Organic & biomolecular chemistry 17 (2019) 1053–1057; doi:10.1039/c8ob02775g

data_7156605
_publ_section_title
;
 Functional characterization of the halogenase SpmH and discovery of new
 deschloro-tryptophan dimers.
;
_journal_issue                   5
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1053
_journal_page_last               1057
_journal_paper_doi               10.1039/c8ob02775g
_journal_volume                  17
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.5(C23 H21 N3 O2)'
_chemical_formula_sum            'C11.5 H10.5 N1.5 O'
_chemical_formula_weight         185.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-10-16 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.1430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.59660(10)
_cell_length_b                   7.86090(10)
_cell_length_c                   11.87830(10)
_cell_measurement_reflns_used    8071
_cell_measurement_temperature    99.97(19)
_cell_measurement_theta_max      73.4240
_cell_measurement_theta_min      4.7320
_cell_volume                     902.899(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(19)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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    -89.00   6.20   0.40    0.40    --    0.00 -19.00   0.00  238
  2  \w    -46.00   4.00   0.40    0.40    --    0.00 -77.00-150.00  125
  3  \w     -5.00  25.00   0.40    0.40    --    0.00 -77.00 150.00   75
  4  \w    -42.00  -8.80   0.40    0.40    --    0.00 -77.00 150.00   83
  5  \w     47.00 118.20   0.40    0.60    --   94.60 -82.00-120.00  178
  6  \w     88.00 127.20   0.40    0.60    --   94.60  77.00-120.00   98
  7  \w     68.00 113.20   0.40    0.60    --   94.60 -45.00-120.00  113
  8  \w    140.00 166.00   0.40    0.60    --   94.60  30.00   0.00   65
  9  \w      7.00  42.20   0.40    0.60    --   94.60 -82.00-120.00   88
 10  \w     34.00  78.00   0.40    0.60    --   94.60 -82.00  30.00  110
 11  \w     46.00  73.20   0.40    0.60    --   94.60 -82.00 150.00   68
 12  \w     91.00 118.20   0.40    0.60    --   94.60 -82.00 150.00   68
 13  \w     78.00 133.20   0.40    0.60    --   94.60  30.00   0.00  138
 14  \w     71.00 182.20   0.40    0.60    --   94.60  61.00-150.00  278
 15  \w      9.00  93.00   0.40    0.60    --   94.60 -61.00-120.00  210
 16  \w    130.00 180.00   0.40    0.60    --   94.60  77.00-120.00  125
 17  \w     73.00 183.00   0.40    0.60    --   94.60  15.00-180.00  275
 18  \w     27.00 106.20   0.40    0.60    --   94.60 -45.00 120.00  198
 19  \w     48.00 124.00   0.40    0.60    --   94.60 -82.00   0.00  190
 20  \w     44.00 119.20   0.40    0.60    --   94.60 -82.00  90.00  188
 21  \w      5.00  43.00   0.40    0.60    --   94.60 -82.00 -60.00   95
 22  \w    100.00 125.20   0.40    0.60    --   94.60 -82.00 -60.00   63
 23  \w     46.00  71.20   0.40    0.60    --   94.60 -77.00  60.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0524552000
_diffrn_orient_matrix_UB_12      -0.0631154000
_diffrn_orient_matrix_UB_13      -0.1342588000
_diffrn_orient_matrix_UB_21      0.0057246000
_diffrn_orient_matrix_UB_22      -0.1849198000
_diffrn_orient_matrix_UB_23      0.0447931000
_diffrn_orient_matrix_UB_31      -0.1503253000
_diffrn_orient_matrix_UB_32      0.0150100000
_diffrn_orient_matrix_UB_33      -0.0130608000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8825
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.733
_diffrn_reflns_theta_min         4.078
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1561 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3527
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.2108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3493
_reflns_number_total             3527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob02775g2.cif
_cod_data_source_block           liuzhiwen_hg-3-(16-17)_collect
_cod_depositor_comments          'Adding full bibliography for 7156605.cif.'
_cod_original_cell_volume        902.898(17)
_cod_original_formula_sum        'C11.50 H10.50 N1.50 O'
_cod_database_code               7156605
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H42 N4 O4 '
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.815
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C00C(H00C), C00I(H00I)
2.b Aromatic/amide H refined with riding coordinates:
 N005(H005), C00E(H00E), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00R(H00R), C00S(H00S)
2.c Idealised Me refined as rotating group:
 C00J(H00A,H00B,H00D), C00P(H00F,H00G,H00H), C00Q(H00J,H00P,H00Q)
2.d Idealised tetrahedral OH refined as rotating group:
 O001(H001)
;
_shelx_res_checksum              17191
_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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.745