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_4129107
_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 H44 Cl Cu N5 O2, 3(C H Cl3)'
_chemical_formula_sum            'C53 H47 Cl10 Cu N5 O2'
_chemical_formula_weight         1203.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                84.5774(17)
_cell_angle_beta                 77.5388(17)
_cell_angle_gamma                67.318(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2842(3)
_cell_length_b                   14.9772(3)
_cell_length_c                   16.2006(3)
_cell_measurement_reflns_used    21969
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.8110
_cell_measurement_theta_min      4.2290
_cell_volume                     2685.11(11)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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     -1.00  25.00   1.00    2.00    --  -34.73  57.00  60.00   26
  2  \w    -42.00 -16.00   1.00    2.00    --  -34.73  57.00  60.00   26
  3  \w     22.00  89.00   1.00    2.00    --   34.73  19.00  90.00   67
  4  \w     73.00  99.00   1.00    2.00    --   34.73  57.00 150.00   26
  5  \w     60.00  87.00   1.00    2.00    --   34.73  77.00  30.00   27
  6  \w     18.00 101.00   1.00    2.00    --   34.73  38.00 -60.00   83
  7  \w    115.00 173.00   1.00    8.00    --  105.88  77.00 -30.00   58
  8  \w    133.00 167.00   1.00    8.00    --  105.88  61.00  60.00   34
  9  \w    124.00 158.00   1.00    8.00    --  105.88  77.00   0.00   34
 10  \w    124.00 156.00   1.00    8.00    --  105.88  77.00 -60.00   32
 11  \w    125.00 173.00   1.00    8.00    --  105.88  77.00 -90.00   48
 12  \w    126.00 171.00   1.00    8.00    --  105.88  77.00-150.00   45
 13  \w    125.00 168.00   1.00    8.00    --  105.88  77.00-120.00   43
 14  \w     89.00 115.00   1.00    8.00    --  105.88  61.00 -90.00   26
 15  \w     88.00 114.00   1.00    8.00    --  105.88  61.00 -60.00   26
 16  \w     88.00 114.00   1.00    8.00    --  105.88  61.00 -30.00   26
 17  \w     86.00 114.00   1.00    8.00    --  105.88  30.00 -60.00   28
 18  \w     79.00 104.00   1.00    8.00    --  105.88  77.00 -30.00   25
 19  \w     79.00 105.00   1.00    8.00    --  105.88  77.00   0.00   26
 20  \w    114.00 173.00   1.00    8.00    --  105.88  77.00  30.00   59
 21  \w    125.00 151.00   1.00    8.00    --  105.88  61.00 120.00   26
 22  \w    120.00 167.00   1.00    8.00    --  105.88  61.00 150.00   47
 23  \w    118.00 172.00   1.00    8.00    --  105.88  77.00  90.00   54
 24  \w     88.00 113.00   1.00    8.00    --  105.88  61.00 120.00   25
 25  \w     88.00 113.00   1.00    8.00    --  105.88  61.00 150.00   25
 26  \w     84.00 109.00   1.00    8.00    --  105.88  30.00 150.00   25
 27  \w     84.00 116.00   1.00    8.00    --  105.88  30.00 120.00   32
 28  \w     84.00 115.00   1.00    8.00    --  105.88  30.00  90.00   31
 29  \w     88.00 113.00   1.00    8.00    --  105.88  61.00  60.00   25
 30  \w     89.00 115.00   1.00    8.00    --  105.88  61.00  90.00   26
 31  \w     84.00 109.00   1.00    8.00    --  105.88  30.00  30.00   25
 32  \w     89.00 115.00   1.00    8.00    --  105.88  61.00  30.00   26
 33  \w     84.00 114.00   1.00    8.00    --  105.88  30.00 -30.00   30
 34  \w     84.00 114.00   1.00    8.00    --  105.88  30.00   0.00   30
 35  \w     79.00 105.00   1.00    8.00    --  105.88  77.00  30.00   26
 36  \w     79.00 105.00   1.00    8.00    --  105.88  77.00  60.00   26
 37  \w     79.00 105.00   1.00    8.00    --  105.88  77.00  90.00   26
 38  \w     79.00 104.00   1.00    8.00    --  105.88  77.00 120.00   25
 39  \w     79.00 105.00   1.00    8.00    --  105.88  77.00 150.00   26
 40  \w     84.00 110.00   1.00    8.00    --  105.88  30.00  60.00   26
 41  \w     79.00 104.00   1.00    8.00    --  105.88  77.00 -60.00   25
 42  \w     79.00 104.00   1.00    8.00    --  105.88  77.00 -90.00   25
 43  \w     79.00 105.00   1.00    8.00    --  105.88  77.00-120.00   26
 44  \w     89.00 115.00   1.00    8.00    --  105.88  61.00-150.00   26
 45  \w     88.00 119.00   1.00    8.00    --  105.88  61.00-180.00   31
 46  \w     85.00 160.00   1.00    8.00    --  105.88  30.00-180.00   75
 47  \w     84.00 111.00   1.00    8.00    --  105.88  30.00-150.00   27
 48  \w     85.00 111.00   1.00    8.00    --  105.88  30.00-120.00   26
 49  \w     85.00 111.00   1.00    8.00    --  105.88  30.00 -90.00   26
 50  \w     79.00 107.00   1.00    8.00    --  105.88  77.00-150.00   28
 51  \w     79.00 172.00   1.00    8.00    --  105.88  77.00-180.00   93
 52  \w     41.00 133.00   1.00    8.00    --  105.88 -77.00 -30.00   92
 53  \w     89.00 114.00   1.00    8.00    --  105.88-111.00  60.00   25
 54  \w     51.00 116.00   1.00    8.00    --  105.88-111.00 150.00   65
 55  \w     38.00  68.00   1.00    8.00    --  105.88-111.00  60.00   30
 56  \w     37.00 100.00   1.00    8.00    --  105.88 -94.00 -60.00   63
 57  \w     38.00 108.00   1.00    8.00    --  105.88 -94.00-120.00   70
 58  \w     37.00  92.00   1.00    8.00    --  105.88 -94.00-180.00   55
 59  \w      1.00  71.00   1.00    2.00    --   34.73 -99.00   0.00   70
 60  \w      1.00  73.00   1.00    2.00    --   34.73 -99.00-120.00   72
 61  \w     17.00  86.00   1.00    2.00    --   34.73  42.00  95.00   69
 62  \w     18.00  70.00   1.00    2.00    --   34.73  57.00 150.00   52
 63  \w      9.00  52.00   1.00    2.00    --   34.73  77.00  30.00   43
 64  \w      8.00 100.00   1.00    2.00    --   34.73  77.00 -30.00   92
 65  \w      8.00 102.00   1.00    2.00    --   34.73  77.00-180.00   94
 66  \w     11.00  62.00   1.00    2.00    --   34.73  77.00-120.00   51
 67  \w    -36.00  63.00   1.00    2.00    --   34.73 -19.00-120.00   99
 68  \w    -34.00  50.00   1.00    2.00    --   34.73 -38.00  30.00   84
 69  \w     36.00  85.00   1.00    2.00    --   34.73-125.00 150.00   49
 70  \w    -34.00  53.00   1.00    2.00    --   34.73 -38.00 120.00   87
 71  \w     -3.00  24.00   1.00    2.00    --   34.73  96.00  94.95   27
;
_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      0.0974771000
_diffrn_orient_matrix_UB_12      -0.0650415000
_diffrn_orient_matrix_UB_13      0.0488692000
_diffrn_orient_matrix_UB_21      -0.0610326000
_diffrn_orient_matrix_UB_22      -0.0743174000
_diffrn_orient_matrix_UB_23      0.0165679000
_diffrn_orient_matrix_UB_31      0.0773327000
_diffrn_orient_matrix_UB_32      -0.0517383000
_diffrn_orient_matrix_UB_33      -0.0826019000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36902
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.522
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83062
_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            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             1230
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0705P)^2^+4.9677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8718
_reflns_number_total             9478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            19Cu.cif
_cod_data_source_block           exp_578
_cod_depositor_comments
'Adding full bibliography for 4129104--4129109.cif.'
_cod_original_cell_volume        2685.10(11)
_cod_database_code               4129107
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C80 N5 H80 Cu1 Cl9 O2'
_shelx_estimated_absorpt_t_max   0.608
_shelx_estimated_absorpt_t_min   0.405
_reflns_odcompleteness_completeness 99.93
_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 Ternary CH refined with riding coordinates:
 C52(H52), C53(H53), C51(H51)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C16(H16), C4(H4), C3(H3), C12(H12), C17(H17), C11(H11), C19(H19),
 C20(H20), C6(H6), C44(H44), C28(H28), C7(H7), C37(H37), C46(H46), C35(H35),
 C26(H26)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C49(H49A,H49B,H49C), C40(H40A,H40B,
 H40C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C32(H32A,H32B,H32C), C50(H50A,
 H50B,H50C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              45965
_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 1.560
_oxdiff_exptl_absorpt_empirical_full_min 0.794