Thienyl MIDA Boronate Esters as Highly Effective Monomers for Suzuki–Miyaura Polymerization Reactions
Carrillo, Josué Ayuso; Ingleson, Michael J.; Turner, Michael L.; Macromolecules 48 (2015) 979–; doi:10.1021/ma502542g

data_1518717
_publ_section_title
;
 Thienyl MIDA Boronate Esters as Highly Effective Monomers for
 Suzuki--Miyaura Polymerization Reactions
;
_journal_issue                   4
_journal_name_full               Macromolecules
_journal_page_first              979
_journal_paper_doi               10.1021/ma502542g
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'C15 H21 B Br N O4 S, C3 H6 O'
_chemical_formula_sum            'C18 H27 B Br N O5 S'
_chemical_formula_weight         460.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
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Olex2 1.2
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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_diffrn_ambient_temperature      150.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.896
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  1 omega  -12.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000  120.0000 105

  2 omega  -12.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000 -120.0000 105

  3 omega  -12.00   93.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.3360   77.0000    0.0000 105
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
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_diffrn_orient_matrix_UB_23      0.0409461000
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_diffrn_orient_matrix_UB_32      -0.0535012000
_diffrn_orient_matrix_UB_33      0.0040467000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.1253
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_diffrn_reflns_number            10504
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_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.027
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_diffrn_source                   'SuperNova (Mo) X-ray Source'
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_exptl_absorpt_correction_T_min  0.62874
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
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_refine_ls_number_reflns         7483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
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_refine_ls_structure_factor_coef Fsqd
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;
 w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+19.9375P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
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_reflns_number_gt                5384
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma502542g_si_002.cif
_cod_data_source_block           amji170_refinalise
_cod_depositor_comments          'Adding full bibliography for 1518717.cif.'
_cod_database_code               1518717
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C16 H21 N1 O4 B1 Br1 S1'
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C29(H29A,H29B), C35(H35A,H35B), C36(H36A,H36B), C41(H41A,H41B),
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2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C44(H44)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C43(H43A,H43B,
 H43C), C47(H47A,H47B,H47C), C52(H52A,H52B,H52C), C1(H1A,H1B,H1C), C2(H2A,H2B,
 H2C)
;
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_olex2_submission_special_instructions 'No special instructions were received'