A General Protocol for the Polycondensation of Thienyl N-Methyliminodiacetic Acid Boronate Esters To Form High Molecular Weight Copolymers.
Carrillo, Josue Ayuso; Turner, Michael L.; Ingleson, Michael J.; Journal of the American Chemical Society 138 (2016) 13361–13368; doi:10.1021/jacs.6b07666

data_4130870
_publ_section_title
;
 A General Protocol for the Polycondensation of Thienyl
 N-Methyliminodiacetic Acid Boronate Esters To Form High Molecular Weight
 Copolymers.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13361
_journal_page_last               13368
_journal_paper_doi               10.1021/jacs.6b07666
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C42 H66 B2 N2 O8 S2, C2 H3 N'
_chemical_formula_sum            'C44 H69 B2 N3 O8 S2'
_chemical_formula_weight         853.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                82.158(3)
_cell_angle_beta                 83.815(3)
_cell_angle_gamma                69.036(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2860(2)
_cell_length_b                   10.6177(4)
_cell_length_c                   28.6890(11)
_cell_measurement_reflns_used    5384
_cell_measurement_temperature    150.02(13)
_cell_measurement_theta_max      28.4600
_cell_measurement_theta_min      3.7000
_cell_volume                     2330.15(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02(13)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details
;
  1 omega  -54.00   63.00   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -19.0000  -60.0000 156

  2 omega   29.00   61.25   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   30.0000 43

  3 omega   45.00   87.00   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -143.0000   36.0000 56

  4 omega   14.00   76.25   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -127.0000 -153.0000 83

  5 omega  -38.00   38.50   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -120.0000 102

  6 omega   14.00   83.00   0.7500   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   57.0000  120.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0059960000
_diffrn_orient_matrix_UB_12      -0.0655256000
_diffrn_orient_matrix_UB_13      0.0108656000
_diffrn_orient_matrix_UB_21      -0.0035459000
_diffrn_orient_matrix_UB_22      0.0219550000
_diffrn_orient_matrix_UB_23      0.0224781000
_diffrn_orient_matrix_UB_31      -0.0915923000
_diffrn_orient_matrix_UB_32      0.0199932000
_diffrn_orient_matrix_UB_33      0.0014384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            19598
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.288
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0419P)^2^+0.9931P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7536
_reflns_number_total             10602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07666_si_002.cif
_cod_data_source_block           amji347
_cod_original_cell_volume        2330.16(15)
_cod_database_code               4130870
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C42H68N2O8S2B2
_reflns_odcompleteness_completeness 99.77
_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:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B),
  C39(H39A,H39B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C40(H40A,H40B,
 H40C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              1505
_shelx_hkl_checksum              30108
_olex2_submission_special_instructions 'No special instructions were received'