Highly nucleophilic dipropanolamine chelated boron reagents for aryl-transmetallation to iron complexes.
Dunsford, Jay J.; Clark, Ewan R.; Ingleson, Michael J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20577–20583; doi:10.1039/c5dt03835a

data_7037573
_publ_section_title
;
 Highly nucleophilic dipropanolamine chelated boron reagents for
 aryl-transmetallation to iron complexes.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20577
_journal_page_last               20583
_journal_paper_doi               10.1039/c5dt03835a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H18 B N O2, H2 O'
_chemical_formula_sum            'C12 H20 B N O3'
_chemical_formula_weight         237.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-06-26 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7171(19)
_cell_length_b                   11.890(2)
_cell_length_c                   11.565(2)
_cell_measurement_temperature    150
_cell_volume                     1222.2(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9888
_diffrn_measured_fraction_theta_max 0.9888
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4143
_diffrn_reflns_theta_full        25.3444
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.2885
_exptl_crystal_description       block
_exptl_crystal_F_000             512.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4644
_refine_diff_density_min         -0.4517
_refine_diff_density_rms         0.1232
_refine_ls_d_res_high            0.8302
_refine_ls_d_res_low             4.9415
_refine_ls_goodness_of_fit_ref   1.0344
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0344
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -6
_reflns_number_gt                1288
_reflns_number_total             2206
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt03835a2.cif
_cod_data_source_block           amji117_refinalise2
_cod_database_code               7037573
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O2(H2a,H2b)
2.b Ternary CH refined with riding coordinates:
 N4(H4)
2.c Secondary CH2 refined with riding coordinates:
 c5(H5a,H5b), c7(H7a,H7b), c8(H8a,H8b), c9(H9a,H9b), c10(H10a,H10b), c12(H12a,
 H12b)
2.d Aromatic/amide H refined with riding coordinates:
 c14(H14), c6(H6), c13(H13), c16(H16), c11(H11)
;