A bioinspired model for copper monooxygenase: direct aromatic hydroxylation using O<sub>2</sub>.
Ramasubramanian, Ramamoorthy; Anandababu, Karunanithi; Kumar, Mukesh; Mayilmurugan, Ramasamy; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8788–8799; doi:10.1039/d4dt02079k

data_7718555
_publ_section_title
;
 A bioinspired model for copper monooxygenase: direct aromatic
 hydroxylation using O<sub>2</sub>.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8788
_journal_page_last               8799
_journal_paper_doi               10.1039/d4dt02079k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C38 H35 Cu2 F6 N6 O8 S2, C F3 O3 S'
_chemical_formula_sum            'C39 H34 Cu2 F9 N6 O11 S3'
_chemical_formula_weight         1156.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-10-31 deposited with the CCDC.	2025-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.7616(6)
_cell_length_b                   10.1552(2)
_cell_length_c                   16.5696(3)
_cell_measurement_reflns_used    7667
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0790
_cell_measurement_theta_min      3.1670
_cell_volume                     4671.38(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    -24.00  66.00   1.00    1.34    --   43.29 -57.00  30.00   90
  2  \w     31.00 119.00   1.00    5.33    --  102.90-126.00 -30.00   88
  3  \w     46.00  88.00   1.00    5.33    --  102.90 -95.00-120.00   42
  4  \w     82.00 150.00   1.00    5.33    --  102.90  45.00-180.00   68
  5  \w     80.00 121.00   1.00    5.33    --  102.90  61.00 -30.00   41
  6  \w     98.00 135.00   1.00    5.33    --  102.90  61.00  90.00   37
  7  \w    -99.00 -72.00   1.00    1.34    --  -43.29-126.00-150.00   27
  8  \w   -118.00 -79.00   1.00    1.34    --  -43.29 -99.00  90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0228283000
_diffrn_orient_matrix_UB_12      -0.0494634000
_diffrn_orient_matrix_UB_13      -0.0577604000
_diffrn_orient_matrix_UB_21      -0.0029222000
_diffrn_orient_matrix_UB_22      -0.0213796000
_diffrn_orient_matrix_UB_23      0.1399850000
_diffrn_orient_matrix_UB_31      -0.0900202000
_diffrn_orient_matrix_UB_32      0.0133032000
_diffrn_orient_matrix_UB_33      0.0101366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12880
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.249
_diffrn_reflns_theta_min         3.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.275
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.728
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 1477 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.00024(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         6944
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0936P)^2^+7.1171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1889
_reflns_Friedel_coverage         0.462
_reflns_Friedel_fraction_full    0.510
_reflns_Friedel_fraction_max     0.486
_reflns_number_gt                6048
_reflns_number_total             6944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02079k2.cif
_cod_data_source_block           rs50_1
_cod_depositor_comments
'Adding full bibliography for 7718555--7718556.cif.'
_cod_database_code               7718555
_chemical_oxdiff_formula         'C39 H34 Cu2 F9 N6 O11 S3'
_reflns_odcompleteness_completeness 99.94
_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. Restrained distances
 O00B-H00B
 0.85 with sigma of 0.01
 O00G-H00G
 0.85 with sigma of 0.01
 S003-H00B
 1.895712 with sigma of 0.02
 Cu02-H00B
 2.666686 with sigma of 0.02
 S005-H00G
 1.901497 with sigma of 0.02
 Cu01-H00G
 2.735298 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C00Q(H00Q), C016(H016)
3.b Aromatic/amide H refined with riding coordinates:
 N00D(H00D), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W),
 C00X(H00X), C00Z(H00Z), C011(H011), C012(H012), C013(H013), C015(H015),
 C017(H017), C018(H018), C019(H019), C01A(H01A), C01C(H01C), C01D(H01D),
 C01E(H01E), C01G(H01G), C01K(H01K), C01N(H01N), C01O(H01O), C01P(H01P),
 C01Q(H01Q)
3.c Idealised Me refined as rotating group:
 C01I(H01B,H01F,H01H), C01L(H01I,H01J,H01L)
;
_shelx_res_checksum              84435
_shelx_hkl_checksum              16873
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-11
_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 2.217
_oxdiff_exptl_absorpt_empirical_full_min 0.268