Alkylammoniotrifluoroborate functionalized polystyrenes: polymeric pre-catalysts for the metal-free borylation of heteroarenes.
Bouchard, Nicolas; Fontaine, Frédéric-Georges; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4846–4856; doi:10.1039/c9dt00484j

data_7049166
_publ_section_title
;
 Alkylammoniotrifluoroborate functionalized polystyrenes: polymeric
 pre-catalysts for the metal-free borylation of heteroarenes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4846
_journal_page_last               4856
_journal_paper_doi               10.1039/c9dt00484j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '4(C10 H13 B F3 N)'
_chemical_formula_sum            'C40 H52 B4 F12 N4'
_chemical_formula_weight         860.09
_chemical_name_common            3-Me
_chemical_name_systematic        3-Me
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-22 deposited with the CCDC.    2019-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.354(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   13.504(3)
_cell_length_b                   10.4434(19)
_cell_length_c                   7.9038(15)
_cell_measurement_reflns_used    2784
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.8392
_cell_measurement_theta_min      2.4954
_cell_volume                     1079.9(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.173
_diffrn_reflns_theta_min         1.556
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0550 before and 0.0449 after correction. The Ratio of minimum to maximum transmission is 0.9088. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_preparation       'Trifluoroborate method'
_exptl_crystal_recrystallization_method 'Slow evaporation in acetone'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3927
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0553P)^2^+0.1210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2611
_reflns_number_total             3927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00484j2.cif
_cod_data_source_block           er20161206_0m
_cod_depositor_comments
'Adding full bibliography for 7049165--7049166.cif.'
_cod_original_cell_volume        1079.9(3)
_cod_database_code               7049166
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Rigid bond restraints
 F3A, F3, F1A, F1, F2A, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1A, F1, F3A, F3, F2A, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1A, F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F2A, F2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F3A, F3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
F1A \\sim F1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F3A \\sim F3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F2 \\sim F2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F2A \\sim F2 \\sim F1 \\sim F1A \\sim F3A \\sim F3: within 3A with sigma of
0.02 and sigma for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 F3A, F1A, F1, F2A, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
;
_olex2_exptl_crystal_mounting_method 'Manual '
_olex2_submission_original_sample_id NB3178
_olex2_submission_special_instructions 'No special instructions were received'