Coerulein B: a water-soluble and water-compatible near-infrared photoredox catalyst.
Tanioka, Masaru; Oyama, Masaya; Nakajima, Kaito; Mori, Minori; Harada, Mei; Matsuya, Yuji; Kamino, Shinichiro; Physical chemistry chemical physics : PCCP 26 (2024) 4474–4479; doi:10.1039/d3cp05585j

data_7247986
_publ_section_title
;
 Coerulein B: a water-soluble and water-compatible near-infrared
 photoredox catalyst.
;
_journal_issue                   5
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              4474
_journal_page_last               4479
_journal_paper_doi               10.1039/d3cp05585j
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C20 H10 O4'
_chemical_formula_sum            'C20 H10 O4'
_chemical_formula_weight         314.28
_chemical_name_systematic        'Coerulein B'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-23
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-06-26 deposited with the CCDC.	2024-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.795(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.7163(5)
_cell_length_b                   11.3800(3)
_cell_length_c                   18.1174(5)
_cell_measurement_reflns_used    3767
_cell_measurement_temperature    103.15
_cell_measurement_theta_max      68.2230
_cell_measurement_theta_min      3.6090
_cell_volume                     2734.21(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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      103.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_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    -32.00  14.00   0.50    1.33    --   41.13 -12.00 -30.00   92
  2  \w    -29.00   4.00   0.50    1.33    --   41.13 -12.00-120.00   66
  3  \w     34.00  69.00   0.50    5.33    --   95.43 -59.00-120.00   70
  4  \w     76.00 107.00   0.50    5.33    --   95.43 -99.00-107.00   62
  5  \w     44.00  77.00   0.50    1.33    --   41.13 -99.00-107.00   66
  6  \w     29.00  57.00   0.50    5.33    --   95.43 -50.00   0.00   56
  7  \w     33.00 100.00   0.50    5.33    --   95.43 -77.00  90.00  134
  8  \w     73.00  99.00   0.50    1.33    --   41.13-138.00  60.00   52
  9  \w     45.00  79.00   0.50    1.33    --   41.13-104.00  90.00   68
 10  \w     31.00  56.00   0.50    5.33    --   95.43 -50.00 150.00   50
 11  \w     28.00  69.00   0.50    5.33    --   95.43 -59.00 150.00   82
 12  \w     29.00  54.00   0.50    5.33    --   95.43 -50.00  90.00   50
 13  \w     29.00  65.00   0.50    5.33    --   95.43 -59.00  90.00   72
 14  \w     30.00 117.00   0.50    5.33    --   95.43-145.00 120.00  174
 15  \w     -3.00  33.00   0.50    1.33    --   41.13-104.00  90.00   72
 16  \w    -22.00  33.00   0.50    1.33    --  -41.44  12.00 -60.00  110
 17  \w    -28.00  26.00   0.50    1.33    --  -41.44  25.00   0.00  108
 18  \w    -39.00  23.00   0.50    1.33    --  -41.44  99.00  -1.00  124
 19  \w    -55.00 -29.00   0.50    5.33    --  -95.75  50.00   0.00   52
 20  \w    -57.00 -32.00   0.50    5.33    --  -95.75  50.00 -30.00   50
 21  \w    -62.00 -28.00   0.50    5.33    --  -95.75  68.00 -30.00   68
 22  \w    -94.00 -23.00   0.50    5.33    --  -95.75  99.00  -1.00  142
 23  \w    -57.00 -32.00   0.50    5.33    --  -95.75  50.00 150.00   50
 24  \w   -130.00-103.00   0.50    5.33    --  -95.75 -99.00-107.00   54
 25  \w    -12.00  40.00   0.50    1.33    --   41.13 -99.00-107.00  104
 26  \w     27.00 106.00   0.50    5.33    --   95.43 -77.00-120.00  158
 27  \w     82.00 118.00   0.50    5.33    --   95.43  42.00-180.00   72
 28  \w    120.00 167.00   0.50    5.33    --   95.43  96.00-150.00   94
 29  \w     84.00 111.00   0.50    5.33    --   95.43  96.00-150.00   54
 30  \w     78.00 125.00   0.50    5.33    --   95.43 117.00-120.00   94
 31  \w     72.00  98.00   0.50    1.33    --   41.13 138.00-120.00   52
 32  \w     82.00 107.00   0.50    1.33    --   41.13 138.00 -90.00   50
 33  \w     91.00 143.00   0.50    5.33    --   95.43  99.00  -1.00  104
 34  \w     84.00 109.00   0.50    1.33    --   41.13 138.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0897331000
_diffrn_orient_matrix_UB_12      0.0742735000
_diffrn_orient_matrix_UB_13      -0.0446622000
_diffrn_orient_matrix_UB_21      -0.0373047000
_diffrn_orient_matrix_UB_22      -0.1046252000
_diffrn_orient_matrix_UB_23      -0.0537903000
_diffrn_orient_matrix_UB_31      -0.0636730000
_diffrn_orient_matrix_UB_32      -0.0432760000
_diffrn_orient_matrix_UB_33      0.0533410000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6756
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.207
_diffrn_reflns_theta_min         4.634
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0605P)^2^+3.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2301
_reflns_number_total             2482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp05585j2.cif
_cod_data_source_block           bx1_1023
_cod_depositor_comments
'Adding full bibliography for 7247986--7247988.cif.'
_cod_database_code               7247986
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C77 H77 O77 '
_diffrn_oxdiff_digest_frames
;
01f238518ce032bfcfec72a16bd5a422f102756ca4a
;
_diffrn_oxdiff_digest_hkl
;
013c79e321185766285f9fd41f9b782164d6ef
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C2(H2), C10(H10), C15(H15), C5(H5), C4(H4), C18(H18), C16(H16),
 C17(H17)
2.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              66003
_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 1.956
_oxdiff_exptl_absorpt_empirical_full_min 0.656