Singly and Doubly Neo-Confused Smaragdyrins.
Rao, Yutao; Zhou, Wenjing; Xu, Ling; Zhou, Mingbo; Yin, Bangshao; Tanaka, Takayuki; Osuka, Atsuhiro; Song, Jianxin; Journal of the American Chemical Society 141 (2019) 18836–18844; doi:10.1021/jacs.9b10270

data_4129109
_publ_section_title
;
 Singly and Doubly Neo-Confused Smaragdyrins.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18836
_journal_page_last               18844
_journal_paper_doi               10.1021/jacs.9b10270
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C50 H46 B F2 N5'
_chemical_formula_sum            'C50 H46 B F2 N5'
_chemical_formula_weight         765.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.90631(13)
_cell_length_b                   16.82151(16)
_cell_length_c                   21.0724(2)
_cell_measurement_reflns_used    27248
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.7570
_cell_measurement_theta_min      4.2540
_cell_volume                     4220.42(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -17.00  30.00   1.00    1.50    --  -34.73  57.00  30.00   47
  2  \w      8.00  65.00   1.00    1.50    --   34.73  77.00 -90.00   57
  3  \w     72.00  99.00   1.00    1.50    --   34.73  77.00-150.00   27
  4  \w     59.00  97.00   1.00    1.50    --   34.73  77.00 -30.00   38
  5  \w     75.00 101.00   1.00    1.50    --   34.73  77.00   0.00   26
  6  \w     66.00 101.00   1.00    1.50    --   34.73  57.00  60.00   35
  7  \w     67.00 100.00   1.00    1.50    --   34.73  38.00   0.00   33
  8  \w     61.00  98.00   1.00    1.50    --   34.73  57.00  90.00   37
  9  \w     59.00 102.00   1.00    1.50    --   34.73  77.00  90.00   43
 10  \w     88.00 114.00   1.00    6.00    --  105.88  61.00   0.00   26
 11  \w    123.00 157.00   1.00    6.00    --  105.88  77.00 -30.00   34
 12  \w    122.00 170.00   1.00    6.00    --  105.88  77.00 -90.00   48
 13  \w    124.00 172.00   1.00    6.00    --  105.88  77.00 -60.00   48
 14  \w    126.00 158.00   1.00    6.00    --  105.88  77.00  30.00   32
 15  \w    124.00 169.00   1.00    6.00    --  105.88  77.00  90.00   45
 16  \w    148.00 173.00   1.00    6.00    --  105.88  61.00 120.00   25
 17  \w    149.00 174.00   1.00    6.00    --  105.88  30.00 120.00   25
 18  \w    111.00 173.00   1.00    6.00    --  105.88  77.00   0.00   62
 19  \w    117.00 173.00   1.00    6.00    --  105.88  77.00-120.00   56
 20  \w    112.00 158.00   1.00    6.00    --  105.88  77.00-180.00   46
 21  \w     88.00 114.00   1.00    6.00    --  105.88  61.00 -60.00   26
 22  \w     88.00 117.00   1.00    6.00    --  105.88  61.00 -30.00   29
 23  \w     84.00 116.00   1.00    6.00    --  105.88  30.00 -30.00   32
 24  \w     88.00 114.00   1.00    6.00    --  105.88  61.00  30.00   26
 25  \w     88.00 114.00   1.00    6.00    --  105.88  61.00  60.00   26
 26  \w     88.00 114.00   1.00    6.00    --  105.88  61.00  90.00   26
 27  \w     88.00 115.00   1.00    6.00    --  105.88  61.00 120.00   27
 28  \w     88.00 114.00   1.00    6.00    --  105.88  61.00 150.00   26
 29  \w     79.00 105.00   1.00    6.00    --  105.88  77.00 120.00   26
 30  \w     79.00 105.00   1.00    6.00    --  105.88  77.00  90.00   26
 31  \w     79.00 173.00   1.00    6.00    --  105.88  77.00  60.00   94
 32  \w     84.00 116.00   1.00    6.00    --  105.88  30.00 120.00   32
 33  \w     84.00 110.00   1.00    6.00    --  105.88  30.00  60.00   26
 34  \w     84.00 115.00   1.00    6.00    --  105.88  30.00  30.00   31
 35  \w     84.00 113.00   1.00    6.00    --  105.88  30.00   0.00   29
 36  \w     79.00 105.00   1.00    6.00    --  105.88  77.00 -30.00   26
 37  \w     79.00 105.00   1.00    6.00    --  105.88  77.00 -60.00   26
 38  \w     79.00 108.00   1.00    6.00    --  105.88  77.00 -90.00   29
 39  \w     79.00 104.00   1.00    6.00    --  105.88  77.00-120.00   25
 40  \w     88.00 167.00   1.00    6.00    --  105.88  61.00-150.00   79
 41  \w     88.00 114.00   1.00    6.00    --  105.88  61.00-180.00   26
 42  \w     79.00 105.00   1.00    6.00    --  105.88  77.00-180.00   26
 43  \w     79.00 105.00   1.00    6.00    --  105.88  77.00-150.00   26
 44  \w     84.00 110.00   1.00    6.00    --  105.88  30.00-150.00   26
 45  \w     85.00 116.00   1.00    6.00    --  105.88  30.00-180.00   31
 46  \w     84.00 118.00   1.00    6.00    --  105.88  30.00 -90.00   34
 47  \w     84.00 110.00   1.00    6.00    --  105.88  30.00 -60.00   26
 48  \w     79.00 105.00   1.00    6.00    --  105.88  77.00   0.00   26
 49  \w     79.00 105.00   1.00    6.00    --  105.88  77.00  30.00   26
 50  \w     84.00 110.00   1.00    6.00    --  105.88  30.00  90.00   26
 51  \w     85.00 110.00   1.00    6.00    --  105.88  30.00 150.00   25
 52  \w     79.00 172.00   1.00    6.00    --  105.88  77.00 150.00   93
 53  \w     89.00 124.00   1.00    6.00    --  105.88 -61.00 -60.00   35
 54  \w     52.00 116.00   1.00    6.00    --  105.88-111.00-180.00   64
 55  \w     39.00  75.00   1.00    6.00    --  105.88 -61.00 -60.00   36
 56  \w     38.00 109.00   1.00    6.00    --  105.88 -94.00 -90.00   71
 57  \w     43.00 106.00   1.00    6.00    --  105.88 -94.00   0.00   63
 58  \w     37.00  96.00   1.00    6.00    --  105.88 -94.00  90.00   59
 59  \w     25.00  88.00   1.00    1.50    --   34.73-125.00 -60.00   63
 60  \w     37.00  85.00   1.00    6.00    --  105.88 -94.00-150.00   48
 61  \w      5.00 102.00   1.00    1.50    --   34.73  19.00 -60.00   97
 62  \w     16.00  57.00   1.00    1.50    --   34.73  38.00   0.00   41
 63  \w     18.00  59.00   1.00    1.50    --   34.73  57.00  60.00   41
 64  \w     18.00  52.00   1.00    1.50    --   34.73  57.00  90.00   34
 65  \w     12.00  71.00   1.00    1.50    --   34.73  77.00   0.00   59
 66  \w      8.00  52.00   1.00    1.50    --   34.73  77.00  90.00   44
 67  \w      9.00 101.00   1.00    1.50    --   34.73  77.00 150.00   92
 68  \w      8.00  48.00   1.00    1.50    --   34.73  77.00 -30.00   40
 69  \w      9.00  64.00   1.00    1.50    --   34.73  77.00-150.00   55
 70  \w    -32.00  50.00   1.00    1.50    --   34.73 -57.00-150.00   82
 71  \w    -29.00  60.00   1.00    1.50    --   34.73 -77.00 -30.00   89
 72  \w      2.00  74.00   1.00    1.50    --   34.73 -99.00  90.00   72
 73  \w    -29.00  51.00   1.00    1.50    --   34.73 -57.00 120.00   80
 74  \w    -50.00 -19.00   1.00    1.50    --  -34.73  57.00  30.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0630964000
_diffrn_orient_matrix_UB_12      0.0780787000
_diffrn_orient_matrix_UB_13      0.0137024000
_diffrn_orient_matrix_UB_21      0.0887333000
_diffrn_orient_matrix_UB_22      0.0464739000
_diffrn_orient_matrix_UB_23      -0.0381541000
_diffrn_orient_matrix_UB_31      -0.0699237000
_diffrn_orient_matrix_UB_32      -0.0115880000
_diffrn_orient_matrix_UB_33      -0.0608174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7442
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         4.265
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;

;
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 3032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.40(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0597P)^2^+1.1357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7109
_reflns_number_total             7442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            15.cif
_cod_data_source_block           exp_521-sr
_cod_depositor_comments
'Adding full bibliography for 4129104--4129109.cif.'
_cod_original_cell_volume        4220.42(8)
_cod_database_code               4129109
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 N5 B1 F2 H100'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.888
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C6(H6), C11(H11), C22(H22), C44(H44), C12(H12), C20(H20), C46(H46),
 C27(H27), C17(H17), C19(H19), C3(H3), C16(H16), C2(H2), C35(H35), C29(H29),
 C8(H8), C9(H9), C37(H37)
2.b Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C50(H50a,H50b,H50c), C49(H49a,H49b,H49c), C26(H26a,H26b,
 H26c), C39(H39a,H39b,H39c), C48(H48a,H48b,H48c), C32(H32a,H32b,H32c), C40(H40a,
 H40b,H40c), C41(H41a,H41b,H41c)
;
_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 1.913
_oxdiff_exptl_absorpt_empirical_full_min 0.664