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_4129106
_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         'C H Cl3, C50 H46 B F2 N5'
_chemical_formula_sum            'C51 H47 B Cl3 F2 N5'
_chemical_formula_weight         885.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-04 deposited with the CCDC.	2019-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.172(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2009(4)
_cell_length_b                   23.2963(16)
_cell_length_c                   21.1770(13)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    99.96(11)
_cell_measurement_theta_max      70.9070
_cell_measurement_theta_min      4.6050
_cell_volume                     4503.7(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(11)
_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    -40.00  -9.00   1.00    5.00    --  -34.73 -19.00 -60.00   31
  2  \w     -7.00  20.00   1.00    5.00    --  -34.73  77.00   0.00   27
  3  \w    -99.00 -59.00   1.00    5.00    --  -34.73 -19.00 -60.00   40
  4  \w    -31.00  -2.00   1.00    5.00    --   34.73 -57.00-150.00   29
  5  \w     53.00 102.00   1.00    5.00    --   34.73  57.00 120.00   49
  6  \w     18.00  79.00   1.00    5.00    --   34.73  57.00  90.00   61
  7  \w     30.00  97.00   1.00    5.00    --   34.73  38.00 -60.00   67
  8  \w    -32.00  50.00   1.00    5.00    --   34.73 -57.00-180.00   82
  9  \w    -33.00  39.00   1.00    5.00    --   34.73 -57.00 -30.00   72
 10  \w     36.00  88.00   1.00    5.00    --   34.73-125.00   0.00   52
 11  \w     33.00  88.00   1.00    5.00    --   34.73-125.00-180.00   55
 12  \w    100.00 162.00   1.00   25.00    --  105.88 111.00-120.00   62
 13  \w     68.00  95.00   1.00   25.00    --  105.88 -94.00 -30.00   27
 14  \w     38.00 123.00   1.00   25.00    --  105.88 -45.00  90.00   85
 15  \w    122.00 173.00   1.00   25.00    --  105.88  77.00 120.00   51
 16  \w     39.00 131.00   1.00   25.00    --  105.88 -77.00-150.00   92
 17  \w    112.00 152.00   1.00   25.00    --  105.88  61.00 -60.00   40
 18  \w     47.00 111.00   1.00   25.00    --  105.88-111.00   0.00   64
 19  \w     37.00 127.00   1.00   25.00    --  105.88 -30.00-180.00   90
 20  \w     58.00 107.00   1.00   25.00    --  105.88 -94.00  60.00   49
 21  \w     41.00 123.00   1.00   25.00    --  105.88 -45.00 -30.00   82
 22  \w     70.00 114.00   1.00   25.00    --  105.88-111.00-150.00   44
 23  \w    124.00 158.00   1.00   25.00    --  105.88   0.00  90.00   34
 24  \w    117.00 159.00   1.00   25.00    --  105.88  45.00-150.00   42
 25  \w     56.00 109.00   1.00   25.00    --  105.88 -94.00 120.00   53
 26  \w     39.00 115.00   1.00   25.00    --  105.88   0.00  90.00   76
;
_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      -0.0882627000
_diffrn_orient_matrix_UB_12      -0.0353970000
_diffrn_orient_matrix_UB_13      0.0434686000
_diffrn_orient_matrix_UB_21      -0.0407367000
_diffrn_orient_matrix_UB_22      0.0555033000
_diffrn_orient_matrix_UB_23      0.0332332000
_diffrn_orient_matrix_UB_31      -0.1379618000
_diffrn_orient_matrix_UB_32      0.0062237000
_diffrn_orient_matrix_UB_33      -0.0488034000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28544
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.795
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62027
_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    1.305
_exptl_crystal_description       needle
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         7941
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1396P)^2^+1.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4992
_reflns_number_total             7941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            13.cif
_cod_data_source_block           exp_722
_cod_depositor_comments
'Adding full bibliography for 4129104--4129109.cif.'
_cod_database_code               4129106
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 N5 H50 B1 F2 Cl3'
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.553
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 Cl1-C7 = Cl02-C7
 1.76 with sigma of 0.02
 Cl1-Cl02
 2.89 with sigma of 0.02
 Cl04-Cl2
 2.89 with sigma of 0.02
 Cl2-C7 = Cl02-C7 = Cl1-C7
 1.76 with sigma of 0.02
 Cl02-Cl2
 2.89 with sigma of 0.02
 Cl02-Cl1
 2.89 with sigma of 0.02
 Cl2-Cl1
 2.89 with sigma of 0.02
 Cl02-C7 = Cl1-C7 = Cl2-C7
 1.76 with sigma of 0.02
 Cl1-C7 = Cl02-C7 = Cl2-C7
 1.76 with sigma of 0.02
 Cl36-Cl04
 2.89 with sigma of 0.02
3. Rigid bond restraints
 Cl2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
5. Others
 Sof(Cl01)=Sof(Cl04)=Sof(C01Q)=Sof(H01)=Sof(Cl36)=1-FVAR(1)
 Sof(Cl02)=Sof(Cl1)=Sof(C7)=Sof(H7)=Sof(Cl2)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C01Q(H01), C7(H7)
6.b Aromatic/amide H refined with riding coordinates:
 N008(H008), N009(H009), C00B(H00B), C00K(H00K), C00Q(H00Q), C00T(H00T),
 C00W(H00W), C00Z(H00Z), C010(H010), C012(H012), C015(H015), C016(H016),
 C019(H019), C01B(H01D), C01C(H01E), C01F(H01I), C01H(H01J), C01I(H01K),
 C01L(H01R)
6.c Idealised Me refined as rotating group:
 C00X(H00A,H00C,H00D), C011(H01A,H01B,H01C), C01D(H01F,H01G,H01H), C01J(H01L,
 H01M,H01N), C01K(H01O,H01P,H01Q), C01M(H01S,H01T,H01U), C01N(H01V,H01W,H01X),
 C01O(H01Y,H,HA), C01P(H01Z,HB,HC)
;
_shelx_res_checksum              10468
_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 1.918
_oxdiff_exptl_absorpt_empirical_full_min 0.456
_ccdc_publ_extra_info
;
Reason for no structure factor data deposited: 
Too large to  include
;