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_7037575
_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         'C26 H24 Cl2 Fe P2'
_chemical_formula_sum            'C26 H24 Cl2 Fe P2'
_chemical_formula_weight         525.18
_chemical_properties_physical    Air-sensitive
_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             2015-04-08
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
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2015-04-09 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.206(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9849(6)
_cell_length_b                   11.4495(7)
_cell_length_c                   16.7344(8)
_cell_measurement_reflns_used    3530
_cell_measurement_temperature    150.0(5)
_cell_measurement_theta_max      28.2260
_cell_measurement_theta_min      3.2320
_cell_volume                     2448.5(2)
_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
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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)
;
_computing_data_reduction
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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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0(5)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.9854
_diffrn_measured_fraction_theta_max 0.8299
_diffrn_measurement_details
;
  1 omega  -65.00  -17.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  100.0000  -37.0000 48

  2 omega  -71.00   53.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798   19.0000  -60.0000 124

  3 omega -103.00  -48.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.1798  178.0000   30.0000 55
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0035915000
_diffrn_orient_matrix_UB_12      0.0618357000
_diffrn_orient_matrix_UB_13      0.0003102000
_diffrn_orient_matrix_UB_21      -0.0077151000
_diffrn_orient_matrix_UB_22      0.0008345000
_diffrn_orient_matrix_UB_23      0.0408990000
_diffrn_orient_matrix_UB_31      0.0548471000
_diffrn_orient_matrix_UB_32      -0.0038997000
_diffrn_orient_matrix_UB_33      0.0134649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9720
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70996
_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    1.4245
_exptl_crystal_description       block
_exptl_crystal_F_000             1083.7048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.1390
_refine_diff_density_min         -1.1223
_refine_diff_density_rms         0.1857
_refine_ls_d_res_high            0.7332
_refine_ls_d_res_low             6.6853
_refine_ls_goodness_of_fit_ref   1.0368
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    46
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0368
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0000P)^2^+4.5845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -16
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -11
_reflns_number_gt                3957
_reflns_number_total             5409
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt03835a2.cif
_cod_data_source_block           amji52
_cod_database_code               7037575
_chemical_oxdiff_formula         'C26 H24 P2 Fe Cl2 Br'
_reflns_odcompleteness_completeness 98.18
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C26(H26), C25(H25),
 C24(H24), C23(H23), C22(H22), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10),
  C11(H11), C12(H12), C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'