A Red Algal Bourbonane Sesquiterpene Synthase Defined by Microgram-scale NMR-coupled Crystalline Sponge XRD Analysis.
Kersten, Roland D.; Lee, Shoukou; Fujita, Daishi; Pluskal, Tomáš; Kram, Susan; Smith, Jennifer E.; Iwai, Takahiro; Noel, Joseph P.; Fujita, Makoto; Weng, Jing-Ke; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09452

data_4126740
_publ_section_title
;
 A Red Algal Bourbonane Sesquiterpene Synthase Defined by Microgram-scale
 NMR-coupled Crystalline Sponge XRD Analysis.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09452
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C87 H72 I12 N24 Zn6'
_chemical_formula_weight         3368.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.030(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.0105(5)
_cell_length_b                   14.9044(2)
_cell_length_c                   31.0306(5)
_cell_measurement_reflns_used    38139
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.7350
_cell_measurement_theta_min      4.1440
_cell_volume                     15836.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'shelXle (Hubschle et al., 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3040
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            78155
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.033
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             6312
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.135
_refine_diff_density_max         1.565
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Flack x determined using 12907 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.057(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1346
_refine_ls_number_reflns         32473
_refine_ls_number_restraints     600
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1047P)^2^+38.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                30603
_reflns_number_total             32473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Dataset_S20_CCDC1533929.cif
_cod_data_source_block           exp_471_b
_cod_database_code               4126740
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.041
_shelx_estimated_absorpt_t_max   0.177
_oxdiff_exptl_absorpt_empirical_full_min 0.509
_oxdiff_exptl_absorpt_empirical_full_max 2.220
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              94124
_shelx_hkl_checksum              53140