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_4129108
_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 H47 N5'
_chemical_formula_sum            'C50 H47 N5'
_chemical_formula_weight         717.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.259(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7390(12)
_cell_length_b                   12.7534(8)
_cell_length_c                   32.675(4)
_cell_measurement_reflns_used    5066
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.6230
_cell_measurement_theta_min      4.0590
_cell_volume                     8590.8(13)
_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  'ShelXL (Sheldrick, 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 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    -53.00  30.00   1.00    4.00    --  -34.48  38.00 150.00   83
  2  \w    -30.00   9.00   1.00    4.00    --   34.48 -77.00  90.00   39
  3  \w     53.00 100.00   1.00    4.00    --   34.48  57.00 -90.00   47
  4  \w      8.00 100.00   1.00    4.00    --   34.48  77.00-150.00   92
  5  \w     33.00  69.00   1.00    4.00    --   34.48-125.00 -30.00   36
  6  \w    -30.00  49.00   1.00    4.00    --   34.48 -57.00   0.00   79
  7  \w      7.00  96.00   1.00    4.00    --   34.48  19.00-150.00   89
  8  \w     64.00  90.00   1.00    4.00    --   34.48-129.00 -66.00   26
  9  \w     23.00  73.00   1.00    4.00    --   34.48 -99.00  90.00   50
 10  \w    -12.00  22.00   1.00    4.00    --   34.48 -57.00 -60.00   34
 11  \w     33.00  74.00   1.00    4.00    --   34.48-125.00  30.00   41
 12  \w     34.00  61.00   1.00    4.00    --   34.48 -77.00  90.00   27
 13  \w     66.00 116.00   1.00   16.00    --  105.88-111.00 150.00   50
 14  \w     75.00 116.00   1.00   16.00    --  105.88 -45.00 -30.00   41
 15  \w     93.00 173.00   1.00   16.00    --  105.88  61.00-180.00   80
 16  \w     59.00 124.00   1.00   16.00    --  105.88 -61.00 120.00   65
 17  \w     39.00 123.00   1.00   16.00    --  105.88 -45.00-150.00   84
 18  \w     49.00 144.00   1.00   16.00    --  105.88 -15.00 120.00   95
 19  \w     56.00 104.00   1.00   16.00    --  105.88 -94.00 -90.00   48
 20  \w     62.00 108.00   1.00   16.00    --  105.88 -94.00 -30.00   46
 21  \w    102.00 162.00   1.00   16.00    --  105.88 111.00 120.00   60
 22  \w     74.00 103.00   1.00   16.00    --  105.88 -94.00-150.00   29
 23  \w     38.00 112.00   1.00   16.00    --  105.88 -45.00  60.00   74
 24  \w     92.00 168.00   1.00   16.00    --  105.88  45.00  90.00   76
 25  \w    120.00 170.00   1.00   16.00    --  105.88 111.00 150.00   50
 26  \w     91.00 139.00   1.00   16.00    --  105.88  77.00 120.00   48
 27  \w     60.00 100.00   1.00   16.00    --  105.88 -94.00  60.00   40
;
_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      0.0391937000
_diffrn_orient_matrix_UB_12      0.0316563000
_diffrn_orient_matrix_UB_13      0.0409257000
_diffrn_orient_matrix_UB_21      0.0535527000
_diffrn_orient_matrix_UB_22      0.0456550000
_diffrn_orient_matrix_UB_23      -0.0239206000
_diffrn_orient_matrix_UB_31      -0.0344057000
_diffrn_orient_matrix_UB_32      0.1072276000
_diffrn_orient_matrix_UB_33      -0.0018784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            7586
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64555
_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    1.110
_exptl_crystal_density_meas      1.110
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0915P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5020
_reflns_number_total             7586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            18.cif
_cod_data_source_block           exp_674-sr
_cod_depositor_comments
'Adding full bibliography for 4129104--4129109.cif.'
_cod_original_cell_volume        8590.7(13)
_cod_database_code               4129108
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 N5 H60 Cl2'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.864
_reflns_odcompleteness_completeness 99.89
_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:
 N3(H3), N1(H1), C23(H23), C13(H13), C18(H18), C12(H12), C17(H17), C10(H10),
 C9(H9), C20(H20), C21(H21), C37(H37), C3(H3A), C4(H4), C8(H8), C28(H28),
 C35(H35), C26(H26), C44(H44), C46(H46)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C49(H49A,H49B,H49C), C30(H30A,H30B,H30C), C39(H39A,H39B,
 H39C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C48(H48A,H48B,H48C), C40(H40A,
 H40B,H40C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              31586
_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 2.049
_oxdiff_exptl_absorpt_empirical_full_min 0.587