Investigation of Hydrophilic Auristatin Derivatives for Use in Antibody Drug Conjugates.
Mendelsohn, Brian A.; Barnscher, Stuart D.; Snyder, Josh T.; An, Zili; Dodd, Jennifer M.; Dugal-Tessier, Julien; Bioconjugate chemistry 28 (2017) 371–381; doi:10.1021/acs.bioconjchem.6b00530

data_1545389
_publ_section_title
;
 Investigation of Hydrophilic Auristatin Derivatives for Use in Antibody
 Drug Conjugates.
;
_journal_issue                   2
_journal_name_full               'Bioconjugate chemistry'
_journal_page_first              371
_journal_page_last               381
_journal_paper_doi               10.1021/acs.bioconjchem.6b00530
_journal_volume                  28
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H65 N6 O6, C2 F3 O2, C2 H3 N'
_chemical_formula_sum            'C41 H68 F3 N7 O8'
_chemical_formula_weight         844.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 93.466(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4629(4)
_cell_length_b                   15.2084(7)
_cell_length_c                   15.6029(6)
_cell_measurement_reflns_used    9634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.34
_cell_measurement_theta_min      4.06
_cell_volume                     2241.39(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18345
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.486
_diffrn_reflns_theta_min         2.837
_diffrn_source                   'I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       platelet
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
; 
 Flack x determined using 3710 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         18345
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0611P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                17660
_reflns_number_total             18345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bc6b00530_si_001.cif
_cod_data_source_block           twin5new
_cod_database_code               1545389
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2014/6
_shelx_res_checksum              1556
_shelx_hkl_checksum              32232