Group 13 complexes of dipyridylmethane, a forgotten ligand in coordination chemistry.
Vasko, Petra; Kinnunen, Virva; O Moilanen, Jani; Roemmele, Tracey L.; Boeré, René T; Konu, Jari; Tuononen, Heikki M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 18247–18259; doi:10.1039/c5dt02830b

data_7036544
_publ_section_title
;
 Group 13 complexes of dipyridylmethane, a forgotten ligand in
 coordination chemistry.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18247
_journal_page_last               18259
_journal_paper_doi               10.1039/c5dt02830b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C11 H10 B2 Cl6 N2'
_chemical_formula_sum            'C11 H10 B2 Cl6 N2'
_chemical_formula_weight         404.53
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-21
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                112.339(5)
_cell_angle_beta                 98.875(5)
_cell_angle_gamma                101.174(5)
_cell_formula_units_Z            2
_cell_length_a                   7.5511(4)
_cell_length_b                   10.7802(6)
_cell_length_c                   11.2368(6)
_cell_measurement_reflns_used    3674
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.6260
_cell_measurement_theta_min      4.3990
_cell_volume                     803.40(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 10.3953
_diffrn_measured_fraction_theta_full 0.9908
_diffrn_measurement_details
;
  1 omega  -49.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9013   37.0000 -150.0000 82

  2 omega   54.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9013 -125.0000 -150.0000 43

  3 omega  -80.00   20.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.5000   61.0000  120.0000 100

  4 omega  -80.00   22.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.5000   61.0000  -30.0000 102

  5 omega -117.00  -80.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -50.5000  -94.0000   90.0000 37

  6 omega   37.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 79

  7 omega   44.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 47

  8 omega   59.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   15.0000  120.0000 117

  9 omega   42.00   78.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 36

 10 omega  105.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000 -180.0000 72

 11 omega   43.00  116.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   90.0000 73

 12 omega   47.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  150.0000 44

 13 omega   36.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000 -150.0000 55

 14 omega   36.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -90.0000 55

 15 omega   36.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 106

 16 omega   44.00  145.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  -90.0000 101
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1250208000
_diffrn_orient_matrix_UB_12      0.1508272000
_diffrn_orient_matrix_UB_13      0.0565374000
_diffrn_orient_matrix_UB_21      -0.1156413000
_diffrn_orient_matrix_UB_22      0.0471545000
_diffrn_orient_matrix_UB_23      0.1020319000
_diffrn_orient_matrix_UB_31      0.1309856000
_diffrn_orient_matrix_UB_32      -0.0294952000
_diffrn_orient_matrix_UB_33      0.0992116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5268
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         4.39
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.675
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.221
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.3046
_exptl_crystal_size_mid          0.1610
_exptl_crystal_size_min          0.0865
_refine_diff_density_max         1.251
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+0.0063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1567
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                2667
_reflns_number_total             2831
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02830b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7036540--7036544.cif.'
_cod_original_cell_volume        803.40(8)
_cod_database_code               7036544
_chemical_oxdiff_formula         'C11 H10 N2 B2 Cl6'
_reflns_odcompleteness_completeness 99.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H9 of C9, H11 of C11, H2 of C2, H10 of C10, H8 of C8, H3 of C3, H4 of C4,
  {H6A,H6B} of C6, H1 of C1
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C3(H3), C8(H8), C10(H10), C2(H2), C11(H11), C9(H9)
;