Discrete and Stereospecific Oligomers Prepared by Sequential and Alternating Single Unit Monomer Insertion.
Huang, Zixuan; Noble, Benjamin B.; Corrigan, Nathaniel; Chu, Yingying; Satoh, Kotaro; Thomas, Donald S.; Hawker, Craig J.; Moad, Graeme; Kamigaito, Masami; Coote, Michelle L.; Boyer, Cyrille; Xu, Jiangtao; Journal of the American Chemical Society 140 (2018) 13392–13406; doi:10.1021/jacs.8b08386

data_4133074
_publ_section_title
;
 Discrete and Stereospecific Oligomers Prepared by Sequential and
 Alternating Single Unit Monomer Insertion.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13392
_journal_page_last               13406
_journal_paper_doi               10.1021/jacs.8b08386
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C21 H19 N O4 S3'
_chemical_formula_sum            'C21 H19 N O4 S3'
_chemical_formula_weight         445.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.53(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.557(4)
_cell_length_b                   5.4170(11)
_cell_length_c                   21.739(4)
_cell_measurement_reflns_used    15010
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.974
_cell_measurement_theta_min      1.067
_cell_volume                     2248.2(8)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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_temperature      100.0
_diffrn_measured_fraction_theta_full 0.818
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4271
_diffrn_reflns_av_unetI/netI     0.4337
_diffrn_reflns_Laue_measured_fraction_full 0.818
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15010
_diffrn_reflns_point_group_measured_fraction_full 0.818
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        22.974
_diffrn_reflns_theta_max         22.974
_diffrn_reflns_theta_min         1.067
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_preparation
'slow diffusion of pentane into dichloromethane'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.3022
_refine_ls_R_factor_gt           0.1801
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4042
_refine_ls_wR_factor_ref         0.4696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1269
_reflns_number_total             2537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08386_si_002.cif
_cod_data_source_block           p21_c_a
_cod_original_cell_volume        2248.1(8)
_cod_database_code               4133074
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C12, C17, C16, C14, C13, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C10, C9, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S3, C18, S2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5 \\sim C4: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13 \\sim C12: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
N1 \\sim C10 \\sim C9 \\sim C8 \\sim C7: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 S1, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C9(H9), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C11(H11A,H11B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4A), C17(H17), C2(H2), C3(H3), C14(H14), C13(H13),
 C15(H15), C16(H16)
5.d Idealised tetrahedral OH refined with riding coordinates:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'